 data_apa1184
_publ_contact_author_name  'Dr. Francesco Capitelli'
_publ_contact_author_address
; CNR - Istituto di Cristallografia (IC)
  v. Salaria Km 29.300 - 00015 Monterotondo (Roma), Italia
;
_publ_contact_author_email    francesco.capitelli@ic.cnr.it
_publ_contact_author_fax     '+39 0690672616'
_publ_contact_author_phone   '+39 0690672630'
_journale_name_full          ?   
_publ_requested_category     FI

loop_
    _publ_author_name
    _publ_author_address
    'Rossi, Manuela'
; Dipartimento di Scienze della Terra, 
 Università degli Studi di Napoli Federico II, 
 Via Mezzocannone 8, 80134 Napoli, Italia
;
    'Ghiara, Maria Rosaria'
; Dipartimento di Scienze della Terra, 
  Università degli Studi di Napoli Federico II, 
Via Mezzocannone 8, 80134 Napoli, Italia
;
    'Chita, Giuseppe'
; CNR - Istituto di Cristallografia (IC)
  v. Amendola 122/o - 70126 Bari, Italia
;
    'Capitelli, Francesco'
; CNR - Istituto di Cristallografia (IC)
  v. Salaria Km 29.300 - 00015 Monterotondo (Roma), Italia
;

 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety           'Ca10 Cl0.25 F1.90 O24 P6'
_chemical_formula_sum
 'Ca10 Cl0.25 F1.90 O24 P6'
_chemical_formula_weight          1015.58
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Ca'  'Ca'   0.2262   0.3064
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            hexagonal
_symmetry_space_group_name_H-M    P63/m
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 '-y, x-y, z'
 'y, -x+y, z+1/2'
 '-x+y, -x, z'
 'x-y, x, z+1/2'
 '-x, -y, -z'
 'x, y, -z-1/2'
 'y, -x+y, -z'
 '-y, x-y, -z-1/2'
 'x-y, x, -z'
 '-x+y, -x, -z-1/2'
 
_cell_length_a                    9.4480(5)
_cell_length_b                    9.4480(5)
_cell_length_c                    6.9040(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 120.00
_cell_volume                      533.72(6)
_cell_formula_units_Z             1
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     167
_cell_measurement_theta_min       3.81
_cell_measurement_theta_max       23.00
 
_exptl_crystal_description        'prism'
_exptl_crystal_colour             'green'
_exptl_crystal_size_max           0.27
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.160
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              503
_exptl_absorpt_coefficient_mu     3.074
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4907
_exptl_absorpt_correction_T_max   0.7486
_exptl_absorpt_process_details    'SADABS'

_exptl_special_details
;
 Sheldrick, G. M. SADABS, Absorption Correction Program. 
 University of Göttingen, Germany, 1996.
; 
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             6839
_diffrn_reflns_av_R_equivalents   0.0307
_diffrn_reflns_av_sigmaI/netI     0.0147
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        8
_diffrn_reflns_theta_min          5.23
_diffrn_reflns_theta_max          27.45
_reflns_number_total              437
_reflns_number_gt                 428
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Collect (Nonius, 1998)'
_computing_data_reduction         'EVALCCD (Duisenberg et al., 2003)'
_computing_cell_refinement        'EVALCCD (Duisenberg et al., 2003)'
_computing_structure_solution     'SIR2008 (Burla et al., 2007)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'DIAMOND 2.1e (1998-2001 Crystal Impact GbR)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'  
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0133P)²+0.5848P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0175(18)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          437
_refine_ls_number_parameters      45
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0165
_refine_ls_R_factor_gt            0.0161
_refine_ls_wR_factor_ref          0.0410
_refine_ls_wR_factor_gt           0.0407
_refine_ls_goodness_of_fit_ref    1.167
_refine_ls_restrained_S_all       1.167
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ca1 Ca 0.6667 0.3333 0.00131(8) 0.01327(17) Uani 1 3 d S . .
Ca2A Ca -0.0065(3) 0.2418(11) 0.2500 0.0111(6) Uani 0.85(6) 2 d SP . .
Ca2B Ca -0.0102(18) 0.265(3) 0.2500 0.0111(6) Uani 0.15(6) 2 d SP . .
P1 P 0.36918(7) 0.39890(7) 0.2500 0.00936(17) Uani 1 2 d S . .
O1 O 0.4850(2) 0.3285(2) 0.2500 0.0144(3) Uani 1 2 d S . .
O2 O 0.4659(2) 0.5876(2) 0.2500 0.0180(4) Uani 1 2 d S . .
O3 O 0.25807(14) 0.34289(17) 0.07039(19) 0.0211(3) Uani 1 1 d . . .
F1 F 0.0000 0.0000 0.2500 0.0521(13) Uani 0.95 6 d SP . .
Cl1 Cl 0.0000 0.0000 0.424(6) 0.118(13) Uiso 0.06 3 d SP . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Ca1 O1 2.4119(12) 3_655 ?
Ca1 O1 2.4119(12) 5_665 ?
Ca1 O1 2.4119(12) . ?
Ca1 O2 2.4643(12) 9 ?
Ca1 O2 2.4643(13) 11_655 ?
Ca1 O2 2.4643(12) 7_665 ?
Ca1 O3 2.8166(14) 11_655 ?
Ca1 O3 2.8166(14) 9 ?
Ca1 O3 2.8166(14) 7_665 ?
Ca1 P1 3.2221(6) 9 ?
Ca1 P1 3.2221(6) 11_655 ?
Ca1 P1 3.2222(6) 7_665 ?
Ca2A F1 2.316(11) . ?
Ca2A O3 2.362(3) 11 ?
Ca2A O3 2.362(3) 6 ?
Ca2A O2 2.398(10) 5_565 ?
Ca2A O3 2.512(3) 8_556 ?
Ca2A O3 2.512(3) . ?
Ca2A Cl1 2.61(2) 8_556 ?
Ca2A Cl1 2.61(2) . ?
Ca2A O1 2.729(5) 3 ?
Ca2A P1 3.088(3) . ?
Ca2A Cl1 3.23(3) 2_554 ?
Ca2A Cl1 3.23(3) 7_556 ?
Ca2B O2 2.20(3) 5_565 ?
Ca2B O3 2.313(6) 11 ?
Ca2B O3 2.313(6) 6 ?
Ca2B F1 2.55(3) . ?
Ca2B O3 2.576(15) 8_556 ?
Ca2B O3 2.576(15) . ?
Ca2B O1 2.648(16) 3 ?
Ca2B Cl1 2.82(3) 8_556 ?
Ca2B Cl1 2.82(3) . ?
Ca2B P1 3.148(16) . ?
Ca2B P1 3.28(3) 5_565 ?
Ca2B P1 3.319(15) 3 ?
P1 O3 1.5376(12) . ?
P1 O3 1.5376(12) 8_556 ?
P1 O1 1.5389(16) . ?
P1 O2 1.5438(17) . ?
P1 Ca1 3.2222(6) 2_665 ?
P1 Ca1 3.2222(6) 7_665 ?
P1 Ca2B 3.28(3) 3_665 ?
P1 Ca2A 3.288(2) 5 ?
P1 Ca2B 3.319(15) 5 ?
P1 Ca2A 3.516(11) 3_665 ?
O1 Ca1 2.4119(12) 8_556 ?
O1 Ca2B 2.648(16) 5 ?
O1 Ca2A 2.729(5) 5 ?
O2 Ca2B 2.20(3) 3_665 ?
O2 Ca2A 2.398(10) 3_665 ?
O2 Ca1 2.4643(12) 7_665 ?
O2 Ca1 2.4643(12) 2_665 ?
O3 Ca2B 2.313(6) 9 ?
O3 Ca2A 2.362(3) 9 ?
O3 Ca1 2.8166(14) 7_665 ?
F1 Cl1 1.20(4) 8_556 ?
F1 Cl1 1.20(4) . ?
F1 Ca2A 2.316(11) 3 ?
F1 Ca2A 2.316(11) 5 ?
F1 Ca2B 2.55(3) 3 ?
F1 Ca2B 2.55(3) 5 ?
Cl1 Cl1 1.05(8) 7_556 ?
Cl1 Cl1 2.41(8) 8_556 ?
Cl1 Ca2A 2.61(2) 3 ?
Cl1 Ca2A 2.61(2) 5 ?
Cl1 Ca2B 2.82(3) 3 ?
Cl1 Ca2B 2.82(3) 5 ?
Cl1 Ca2A 3.23(3) 9_556 ?
Cl1 Ca2A 3.23(3) 7_556 ?
Cl1 Ca2A 3.23(3) 11_556 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 Ca1 O1 74.92(4) 3_655 5_665 ?
O1 Ca1 O1 74.92(4) 3_655 . ?
O1 Ca1 O1 74.92(4) 5_665 . ?
O1 Ca1 O2 92.43(4) 3_655 9 ?
O1 Ca1 O2 154.13(5) 5_665 9 ?
O1 Ca1 O2 124.16(5) . 9 ?
O1 Ca1 O2 124.16(5) 3_655 11_655 ?
O1 Ca1 O2 92.43(4) 5_665 11_655 ?
O1 Ca1 O2 154.13(5) . 11_655 ?
O2 Ca1 O2 75.90(5) 9 11_655 ?
O1 Ca1 O2 154.13(5) 3_655 7_665 ?
O1 Ca1 O2 124.16(5) 5_665 7_665 ?
O1 Ca1 O2 92.43(4) . 7_665 ?
O2 Ca1 O2 75.90(4) 9 7_665 ?
O2 Ca1 O2 75.90(4) 11_655 7_665 ?
O1 Ca1 O3 69.10(4) 3_655 11_655 ?
O1 Ca1 O3 86.37(5) 5_665 11_655 ?
O1 Ca1 O3 142.70(4) . 11_655 ?
O2 Ca1 O3 67.94(5) 9 11_655 ?
O2 Ca1 O3 55.77(4) 11_655 11_655 ?
O2 Ca1 O3 124.54(4) 7_665 11_655 ?
O1 Ca1 O3 86.37(5) 3_655 9 ?
O1 Ca1 O3 142.70(4) 5_665 9 ?
O1 Ca1 O3 69.10(4) . 9 ?
O2 Ca1 O3 55.77(4) 9 9 ?
O2 Ca1 O3 124.54(4) 11_655 9 ?
O2 Ca1 O3 67.94(5) 7_665 9 ?
O3 Ca1 O3 116.980(16) 11_655 9 ?
O1 Ca1 O3 142.70(4) 3_655 7_665 ?
O1 Ca1 O3 69.10(4) 5_665 7_665 ?
O1 Ca1 O3 86.37(5) . 7_665 ?
O2 Ca1 O3 124.54(4) 9 7_665 ?
O2 Ca1 O3 67.94(5) 11_655 7_665 ?
O2 Ca1 O3 55.77(4) 7_665 7_665 ?
O3 Ca1 O3 116.980(16) 11_655 7_665 ?
O3 Ca1 O3 116.979(16) 9 7_665 ?
O1 Ca1 P1 92.59(3) 3_655 9 ?
O1 Ca1 P1 166.66(3) 5_665 9 ?
O1 Ca1 P1 97.58(4) . 9 ?
O2 Ca1 P1 27.61(4) 9 9 ?
O2 Ca1 P1 98.61(3) 11_655 9 ?
O2 Ca1 P1 66.36(4) 7_665 9 ?
O3 Ca1 P1 93.62(3) 11_655 9 ?
O3 Ca1 P1 28.50(3) 9 9 ?
O3 Ca1 P1 122.12(3) 7_665 9 ?
O1 Ca1 P1 97.58(4) 3_655 11_655 ?
O1 Ca1 P1 92.59(3) 5_665 11_655 ?
O1 Ca1 P1 166.66(3) . 11_655 ?
O2 Ca1 P1 66.36(4) 9 11_655 ?
O2 Ca1 P1 27.61(4) 11_655 11_655 ?
O2 Ca1 P1 98.61(3) 7_665 11_655 ?
O3 Ca1 P1 28.50(3) 11_655 11_655 ?
O3 Ca1 P1 122.12(3) 9 11_655 ?
O3 Ca1 P1 93.62(3) 7_665 11_655 ?
P1 Ca1 P1 93.731(14) 9 11_655 ?
O1 Ca1 P1 166.66(3) 3_655 7_665 ?
O1 Ca1 P1 97.58(4) 5_665 7_665 ?
O1 Ca1 P1 92.59(3) . 7_665 ?
O2 Ca1 P1 98.61(3) 9 7_665 ?
O2 Ca1 P1 66.36(4) 11_655 7_665 ?
O2 Ca1 P1 27.61(4) 7_665 7_665 ?
O3 Ca1 P1 122.12(3) 11_655 7_665 ?
O3 Ca1 P1 93.62(3) 9 7_665 ?
O3 Ca1 P1 28.50(3) 7_665 7_665 ?
P1 Ca1 P1 93.731(14) 9 7_665 ?
P1 Ca1 P1 93.731(14) 11_655 7_665 ?
F1 Ca2A O3 103.2(3) . 11 ?
F1 Ca2A O3 103.2(3) . 6 ?
O3 Ca2A O3 139.0(4) 11 6 ?
F1 Ca2A O2 152.7(2) . 5_565 ?
O3 Ca2A O2 85.4(3) 11 5_565 ?
O3 Ca2A O2 85.4(3) 6 5_565 ?
F1 Ca2A O3 82.1(3) . 8_556 ?
O3 Ca2A O3 136.23(9) 11 8_556 ?
O3 Ca2A O3 78.32(4) 6 8_556 ?
O2 Ca2A O3 74.25(13) 5_565 8_556 ?
F1 Ca2A O3 82.1(3) . . ?
O3 Ca2A O3 78.32(4) 11 . ?
O3 Ca2A O3 136.23(9) 6 . ?
O2 Ca2A O3 74.25(13) 5_565 . ?
O3 Ca2A O3 59.15(10) 8_556 . ?
F1 Ca2A Cl1 27.4(8) . 8_556 ?
O3 Ca2A Cl1 76.7(8) 11 8_556 ?
O3 Ca2A Cl1 129.3(8) 6 8_556 ?
O2 Ca2A Cl1 142.1(6) 5_565 8_556 ?
O3 Ca2A Cl1 96.1(5) 8_556 8_556 ?
O3 Ca2A Cl1 69.6(4) . 8_556 ?
F1 Ca2A Cl1 27.4(8) . . ?
O3 Ca2A Cl1 129.3(8) 11 . ?
O3 Ca2A Cl1 76.7(8) 6 . ?
O2 Ca2A Cl1 142.1(6) 5_565 . ?
O3 Ca2A Cl1 69.6(4) 8_556 . ?
O3 Ca2A Cl1 96.1(5) . . ?
Cl1 Ca2A Cl1 54.9(16) 8_556 . ?
F1 Ca2A O1 106.5(2) . 3 ?
O3 Ca2A O1 71.35(13) 11 3 ?
O3 Ca2A O1 71.35(13) 6 3 ?
O2 Ca2A O1 100.8(4) 5_565 3 ?
O3 Ca2A O1 149.59(15) 8_556 3 ?
O3 Ca2A O1 149.59(15) . 3 ?
Cl1 Ca2A O1 104.6(2) 8_556 3 ?
Cl1 Ca2A O1 104.6(2) . 3 ?
F1 Ca2A P1 83.3(2) . . ?
O3 Ca2A P1 106.91(6) 11 . ?
O3 Ca2A P1 106.91(6) 6 . ?
O2 Ca2A P1 69.46(9) 5_565 . ?
O3 Ca2A P1 29.66(5) 8_556 . ?
O3 Ca2A P1 29.66(5) . . ?
Cl1 Ca2A P1 84.0(2) 8_556 . ?
Cl1 Ca2A P1 84.0(2) . . ?
O1 Ca2A P1 170.2(4) 3 . ?
F1 Ca2A Cl1 44.2(6) . 2_554 ?
O3 Ca2A Cl1 60.7(5) 11 2_554 ?
O3 Ca2A Cl1 144.7(6) 6 2_554 ?
O2 Ca2A Cl1 129.6(4) 5_565 2_554 ?
O3 Ca2A Cl1 104.2(4) 8_556 2_554 ?
O3 Ca2A Cl1 63.7(2) . 2_554 ?
Cl1 Ca2A Cl1 16.7(14) 8_556 2_554 ?
Cl1 Ca2A Cl1 71.6(4) . 2_554 ?
O1 Ca2A Cl1 101.76(16) 3 2_554 ?
P1 Ca2A Cl1 85.18(19) . 2_554 ?
F1 Ca2A Cl1 44.2(6) . 7_556 ?
O3 Ca2A Cl1 144.7(6) 11 7_556 ?
O3 Ca2A Cl1 60.7(5) 6 7_556 ?
O2 Ca2A Cl1 129.6(4) 5_565 7_556 ?
O3 Ca2A Cl1 63.7(2) 8_556 7_556 ?
O3 Ca2A Cl1 104.2(4) . 7_556 ?
Cl1 Ca2A Cl1 71.6(4) 8_556 7_556 ?
Cl1 Ca2A Cl1 16.7(14) . 7_556 ?
O1 Ca2A Cl1 101.76(16) 3 7_556 ?
P1 Ca2A Cl1 85.18(19) . 7_556 ?
Cl1 Ca2A Cl1 88.3(11) 2_554 7_556 ?
O2 Ca2B O3 91.2(8) 5_565 11 ?
O2 Ca2B O3 91.2(8) 5_565 6 ?
O3 Ca2B O3 146.1(9) 11 6 ?
O2 Ca2B F1 148.8(8) 5_565 . ?
O3 Ca2B F1 97.6(7) 11 . ?
O3 Ca2B F1 97.6(7) 6 . ?
O2 Ca2B O3 76.3(4) 5_565 8_556 ?
O3 Ca2B O3 135.3(5) 11 8_556 ?
O3 Ca2B O3 77.9(2) 6 8_556 ?
F1 Ca2B O3 76.5(7) . 8_556 ?
O2 Ca2B O3 76.3(4) 5_565 . ?
O3 Ca2B O3 77.9(2) 11 . ?
O3 Ca2B O3 135.3(5) 6 . ?
F1 Ca2B O3 76.5(7) . . ?
O3 Ca2B O3 57.5(4) 8_556 . ?
O2 Ca2B O1 108.9(11) 5_565 3 ?
O3 Ca2B O1 73.6(4) 11 3 ?
O3 Ca2B O1 73.6(4) 6 3 ?
F1 Ca2B O1 102.3(7) . 3 ?
O3 Ca2B O1 151.07(17) 8_556 3 ?
O3 Ca2B O1 151.07(17) . 3 ?
O2 Ca2B Cl1 140.7(7) 5_565 8_556 ?
O3 Ca2B Cl1 73.3(9) 11 8_556 ?
O3 Ca2B Cl1 121.8(12) 6 8_556 ?
F1 Ca2B Cl1 25.2(8) . 8_556 ?
O3 Ca2B Cl1 89.6(9) 8_556 8_556 ?
O3 Ca2B Cl1 65.4(6) . 8_556 ?
O1 Ca2B Cl1 101.1(6) 3 8_556 ?
O2 Ca2B Cl1 140.7(7) 5_565 . ?
O3 Ca2B Cl1 121.8(12) 11 . ?
O3 Ca2B Cl1 73.3(9) 6 . ?
F1 Ca2B Cl1 25.2(8) . . ?
O3 Ca2B Cl1 65.4(6) 8_556 . ?
O3 Ca2B Cl1 89.6(9) . . ?
O1 Ca2B Cl1 101.1(6) 3 . ?
Cl1 Ca2B Cl1 50.4(16) 8_556 . ?
O2 Ca2B P1 70.3(4) 5_565 . ?
O3 Ca2B P1 106.3(4) 11 . ?
O3 Ca2B P1 106.3(4) 6 . ?
F1 Ca2B P1 78.5(6) . . ?
O3 Ca2B P1 29.02(17) 8_556 . ?
O3 Ca2B P1 29.02(17) . . ?
O1 Ca2B P1 179.2(12) 3 . ?
Cl1 Ca2B P1 79.6(6) 8_556 . ?
Cl1 Ca2B P1 79.6(6) . . ?
O2 Ca2B P1 23.6(4) 5_565 5_565 ?
O3 Ca2B P1 84.4(8) 11 5_565 ?
O3 Ca2B P1 84.4(8) 6 5_565 ?
F1 Ca2B P1 172.4(6) . 5_565 ?
O3 Ca2B P1 96.9(6) 8_556 5_565 ?
O3 Ca2B P1 96.9(6) . 5_565 ?
O1 Ca2B P1 85.3(7) 3 5_565 ?
Cl1 Ca2B P1 153.7(8) 8_556 5_565 ?
Cl1 Ca2B P1 153.7(8) . 5_565 ?
P1 Ca2B P1 93.9(5) . 5_565 ?
O2 Ca2B P1 135.9(10) 5_565 3 ?
O3 Ca2B P1 77.4(4) 11 3 ?
O3 Ca2B P1 77.4(4) 6 3 ?
F1 Ca2B P1 75.3(5) . 3 ?
O3 Ca2B P1 139.2(8) 8_556 3 ?
O3 Ca2B P1 139.2(8) . 3 ?
O1 Ca2B P1 27.01(18) 3 3 ?
Cl1 Ca2B P1 76.7(5) 8_556 3 ?
Cl1 Ca2B P1 76.7(5) . 3 ?
P1 Ca2B P1 153.8(10) . 3 ?
P1 Ca2B P1 112.3(7) 5_565 3 ?
O3 P1 O3 107.51(10) . 8_556 ?
O3 P1 O1 111.22(6) . . ?
O3 P1 O1 111.22(6) 8_556 . ?
O3 P1 O2 107.78(7) . . ?
O3 P1 O2 107.78(7) 8_556 . ?
O1 P1 O2 111.17(10) . . ?
O3 P1 Ca2A 53.96(5) . . ?
O3 P1 Ca2A 53.96(5) 8_556 . ?
O1 P1 Ca2A 133.4(2) . . ?
O2 P1 Ca2A 115.4(2) . . ?
O3 P1 Ca2B 54.38(8) . . ?
O3 P1 Ca2B 54.38(8) 8_556 . ?
O1 P1 Ca2B 137.7(5) . . ?
O2 P1 Ca2B 111.2(5) . . ?
Ca2A P1 Ca2B 4.2(4) . . ?
O3 P1 Ca1 112.51(5) . 2_665 ?
O3 P1 Ca1 60.94(5) 8_556 2_665 ?
O1 P1 Ca1 135.73(5) . 2_665 ?
O2 P1 Ca1 47.72(4) . 2_665 ?
Ca2A P1 Ca1 80.24(17) . 2_665 ?
Ca2B P1 Ca1 76.7(4) . 2_665 ?
O3 P1 Ca1 60.94(5) . 7_665 ?
O3 P1 Ca1 112.51(5) 8_556 7_665 ?
O1 P1 Ca1 135.73(5) . 7_665 ?
O2 P1 Ca1 47.72(4) . 7_665 ?
Ca2A P1 Ca1 80.24(17) . 7_665 ?
Ca2B P1 Ca1 76.7(4) . 7_665 ?
Ca1 P1 Ca1 65.16(2) 2_665 7_665 ?
O3 P1 Ca2B 122.69(10) . 3_665 ?
O3 P1 Ca2B 122.69(10) 8_556 3_665 ?
O1 P1 Ca2B 76.3(3) . 3_665 ?
O2 P1 Ca2B 34.9(3) . 3_665 ?
Ca2A P1 Ca2B 150.3(3) . 3_665 ?
Ca2B P1 Ca2B 146.1(5) . 3_665 ?
Ca1 P1 Ca2B 74.8(2) 2_665 3_665 ?
Ca1 P1 Ca2B 74.8(2) 7_665 3_665 ?
O3 P1 Ca2A 79.61(12) . 5 ?
O3 P1 Ca2A 79.61(12) 8_556 5 ?
O1 P1 Ca2A 55.5(2) . 5 ?
O2 P1 Ca2A 166.7(2) . 5 ?
Ca2A P1 Ca2A 77.9(4) . 5 ?
Ca2B P1 Ca2A 82.1(7) . 5 ?
Ca1 P1 Ca2A 140.50(11) 2_665 5 ?
Ca1 P1 Ca2A 140.50(11) 7_665 5 ?
Ca2B P1 Ca2A 131.8(4) 3_665 5 ?
O3 P1 Ca2B 82.0(3) . 5 ?
O3 P1 Ca2B 82.0(3) 8_556 5 ?
O1 P1 Ca2B 51.4(5) . 5 ?
O2 P1 Ca2B 162.6(5) . 5 ?
Ca2A P1 Ca2B 82.0(7) . 5 ?
Ca2B P1 Ca2B 86.2(10) . 5 ?
Ca1 P1 Ca2B 142.5(2) 2_665 5 ?
Ca1 P1 Ca2B 142.5(2) 7_665 5 ?
Ca2B P1 Ca2B 127.7(7) 3_665 5 ?
Ca2A P1 Ca2B 4.1(3) 5 5 ?
O3 P1 Ca2A 122.43(6) . 3_665 ?
O3 P1 Ca2A 122.43(6) 8_556 3_665 ?
O1 P1 Ca2A 77.16(9) . 3_665 ?
O2 P1 Ca2A 34.01(8) . 3_665 ?
Ca2A P1 Ca2A 149.43(17) . 3_665 ?
Ca2B P1 Ca2A 145.2(5) . 3_665 ?
Ca1 P1 Ca2A 74.11(4) 2_665 3_665 ?
Ca1 P1 Ca2A 74.11(4) 7_665 3_665 ?
Ca2B P1 Ca2A 0.9(3) 3_665 3_665 ?
Ca2A P1 Ca2A 132.7(2) 5 3_665 ?
Ca2B P1 Ca2A 128.6(5) 5 3_665 ?
P1 O1 Ca1 130.15(5) . 8_556 ?
P1 O1 Ca1 130.15(5) . . ?
Ca1 O1 Ca1 90.77(6) 8_556 . ?
P1 O1 Ca2B 101.6(6) . 5 ?
Ca1 O1 Ca2B 98.2(4) 8_556 5 ?
Ca1 O1 Ca2B 98.2(4) . 5 ?
P1 O1 Ca2A 96.8(2) . 5 ?
Ca1 O1 Ca2A 101.53(16) 8_556 5 ?
Ca1 O1 Ca2A 101.53(16) . 5 ?
Ca2B O1 Ca2A 4.8(5) 5 5 ?
P1 O2 Ca2B 121.5(6) . 3_665 ?
P1 O2 Ca2A 124.88(18) . 3_665 ?
Ca2B O2 Ca2A 3.4(5) 3_665 3_665 ?
P1 O2 Ca1 104.67(6) . 7_665 ?
Ca2B O2 Ca1 115.7(3) 3_665 7_665 ?
Ca2A O2 Ca1 113.55(11) 3_665 7_665 ?
P1 O2 Ca1 104.67(6) . 2_665 ?
Ca2B O2 Ca1 115.7(3) 3_665 2_665 ?
Ca2A O2 Ca1 113.55(11) 3_665 2_665 ?
Ca1 O2 Ca1 89.51(6) 7_665 2_665 ?
P1 O3 Ca2B 139.3(5) . 9 ?
P1 O3 Ca2A 142.15(15) . 9 ?
Ca2B O3 Ca2A 5.7(5) 9 9 ?
P1 O3 Ca2A 96.38(7) . . ?
Ca2B O3 Ca2A 121.8(7) 9 . ?
Ca2A O3 Ca2A 117.0(3) 9 . ?
P1 O3 Ca2B 96.60(17) . . ?
Ca2B O3 Ca2B 122.8(8) 9 . ?
Ca2A O3 Ca2B 118.3(4) 9 . ?
Ca2A O3 Ca2B 5.2(4) . . ?
P1 O3 Ca1 90.56(6) . 7_665 ?
Ca2B O3 Ca1 96.1(6) 9 7_665 ?
Ca2A O3 Ca1 100.3(2) 9 7_665 ?
Ca2A O3 Ca1 99.3(3) . 7_665 ?
Ca2B O3 Ca1 94.2(6) . 7_665 ?
Cl1 F1 Cl1 180.000(6) 8_556 . ?
Cl1 F1 Ca2A 90.000(4) 8_556 3 ?
Cl1 F1 Ca2A 90.000(4) . 3 ?
Cl1 F1 Ca2A 90.000(2) 8_556 5 ?
Cl1 F1 Ca2A 90.000(2) . 5 ?
Ca2A F1 Ca2A 120.0 3 5 ?
Cl1 F1 Ca2A 90.000(2) 8_556 . ?
Cl1 F1 Ca2A 90.000(2) . . ?
Ca2A F1 Ca2A 120.0 3 . ?
Ca2A F1 Ca2A 120.0 5 . ?
Cl1 F1 Ca2B 90.000(5) 8_556 3 ?
Cl1 F1 Ca2B 90.000(5) . 3 ?
Ca2A F1 Ca2B 0.5(4) 3 3 ?
Ca2A F1 Ca2B 119.5(4) 5 3 ?
Ca2A F1 Ca2B 120.5(4) . 3 ?
Cl1 F1 Ca2B 90.000(2) 8_556 5 ?
Cl1 F1 Ca2B 90.000(2) . 5 ?
Ca2A F1 Ca2B 120.5(4) 3 5 ?
Ca2A F1 Ca2B 0.5(4) 5 5 ?
Ca2A F1 Ca2B 119.5(4) . 5 ?
Ca2B F1 Ca2B 120.000(1) 3 5 ?
Cl1 F1 Ca2B 90.000(2) 8_556 . ?
Cl1 F1 Ca2B 90.000(2) . . ?
Ca2A F1 Ca2B 119.5(4) 3 . ?
Ca2A F1 Ca2B 120.5(4) 5 . ?
Ca2A F1 Ca2B 0.5(4) . . ?
Ca2B F1 Ca2B 120.000(1) 3 . ?
Ca2B F1 Ca2B 120.000(2) 5 . ?
Cl1 Cl1 F1 180.000(9) 7_556 . ?
Cl1 Cl1 Cl1 180.000(19) 7_556 8_556 ?
F1 Cl1 Cl1 0.000(3) . 8_556 ?
Cl1 Cl1 Ca2A 117.4(8) 7_556 3 ?
F1 Cl1 Ca2A 62.6(8) . 3 ?
Cl1 Cl1 Ca2A 62.6(8) 8_556 3 ?
Cl1 Cl1 Ca2A 117.4(8) 7_556 5 ?
F1 Cl1 Ca2A 62.6(8) . 5 ?
Cl1 Cl1 Ca2A 62.6(8) 8_556 5 ?
Ca2A Cl1 Ca2A 100.5(10) 3 5 ?
Cl1 Cl1 Ca2A 117.4(8) 7_556 . ?
F1 Cl1 Ca2A 62.6(8) . . ?
Cl1 Cl1 Ca2A 62.6(8) 8_556 . ?
Ca2A Cl1 Ca2A 100.5(10) 3 . ?
Ca2A Cl1 Ca2A 100.5(10) 5 . ?
Cl1 Cl1 Ca2B 115.2(8) 7_556 3 ?
F1 Cl1 Ca2B 64.8(8) . 3 ?
Cl1 Cl1 Ca2B 64.8(8) 8_556 3 ?
Ca2A Cl1 Ca2B 2.27(19) 3 3 ?
Ca2A Cl1 Ca2B 101.4(10) 5 3 ?
Ca2A Cl1 Ca2B 102.2(10) . 3 ?
Cl1 Cl1 Ca2B 115.2(8) 7_556 5 ?
F1 Cl1 Ca2B 64.8(8) . 5 ?
Cl1 Cl1 Ca2B 64.8(8) 8_556 5 ?
Ca2A Cl1 Ca2B 102.2(10) 3 5 ?
Ca2A Cl1 Ca2B 2.27(18) 5 5 ?
Ca2A Cl1 Ca2B 101.4(10) . 5 ?
Ca2B Cl1 Ca2B 103.2(10) 3 5 ?
Cl1 Cl1 Ca2B 115.2(8) 7_556 . ?
F1 Cl1 Ca2B 64.8(8) . . ?
Cl1 Cl1 Ca2B 64.8(8) 8_556 . ?
Ca2A Cl1 Ca2B 101.4(10) 3 . ?
Ca2A Cl1 Ca2B 102.2(10) 5 . ?
Ca2A Cl1 Ca2B 2.27(18) . . ?
Ca2B Cl1 Ca2B 103.2(10) 3 . ?
Ca2B Cl1 Ca2B 103.2(10) 5 . ?
Cl1 Cl1 Ca2A 45.8(6) 7_556 9_556 ?
F1 Cl1 Ca2A 134.2(6) . 9_556 ?
Cl1 Cl1 Ca2A 134.2(6) 8_556 9_556 ?
Ca2A Cl1 Ca2A 163.3(14) 3 9_556 ?
Ca2A Cl1 Ca2A 90.2(3) 5 9_556 ?
Ca2A Cl1 Ca2A 90.2(3) . 9_556 ?
Ca2B Cl1 Ca2A 161.1(13) 3 9_556 ?
Ca2B Cl1 Ca2A 88.1(4) 5 9_556 ?
Ca2B Cl1 Ca2A 88.7(4) . 9_556 ?
Cl1 Cl1 Ca2A 45.8(6) 7_556 7_556 ?
F1 Cl1 Ca2A 134.2(6) . 7_556 ?
Cl1 Cl1 Ca2A 134.2(6) 8_556 7_556 ?
Ca2A Cl1 Ca2A 90.2(3) 3 7_556 ?
Ca2A Cl1 Ca2A 90.2(3) 5 7_556 ?
Ca2A Cl1 Ca2A 163.3(14) . 7_556 ?
Ca2B Cl1 Ca2A 88.1(4) 3 7_556 ?
Ca2B Cl1 Ca2A 88.7(4) 5 7_556 ?
Ca2B Cl1 Ca2A 161.1(13) . 7_556 ?
Ca2A Cl1 Ca2A 76.8(9) 9_556 7_556 ?
Cl1 Cl1 Ca2A 45.8(6) 7_556 11_556 ?
F1 Cl1 Ca2A 134.2(6) . 11_556 ?
Cl1 Cl1 Ca2A 134.2(6) 8_556 11_556 ?
Ca2A Cl1 Ca2A 90.2(3) 3 11_556 ?
Ca2A Cl1 Ca2A 163.3(14) 5 11_556 ?
Ca2A Cl1 Ca2A 90.2(3) . 11_556 ?
Ca2B Cl1 Ca2A 88.7(4) 3 11_556 ?
Ca2B Cl1 Ca2A 161.1(13) 5 11_556 ?
Ca2B Cl1 Ca2A 88.1(4) . 11_556 ?
Ca2A Cl1 Ca2A 76.8(9) 9_556 11_556 ?
Ca2A Cl1 Ca2A 76.8(9) 7_556 11_556 ?
 
_diffrn_measured_fraction_theta_max    0.986
_diffrn_reflns_theta_full              27.45
_diffrn_measured_fraction_theta_full   0.986
_refine_diff_density_max    0.319
_refine_diff_density_min   -0.416
_refine_diff_density_rms    0.068

