 
data_gyp_xxa_2p7
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 gypsum-II
;
_chemical_name_common             gypsum
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Ca O6 S'
_chemical_formula_weight          168.14
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Ca'  'Ca'   0.1611   0.1926
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0056   0.0036
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.0826   0.0763
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    'P 21/n'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    5.865(12)
_cell_length_b                    15.045(14)
_cell_length_c                    5.478(12)
_cell_angle_alpha                 90.00
_cell_angle_beta                  115.3(2)
_cell_angle_gamma                 90.00
_cell_volume                      437.0(14)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     211
_cell_measurement_theta_min       5.02
_cell_measurement_theta_max       13.78
 
_exptl_crystal_description        block
_exptl_crystal_colour             white
_exptl_crystal_size_max           0.09
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.556
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              336
_exptl_absorpt_coefficient_mu     0.941
_exptl_absorpt_correction_type    'gaussian'
_exptl_absorpt_correction_T_min   0.230
_exptl_absorpt_correction_T_max   0.451
_exptl_absorpt_process_details    'ABSPACK (Oxford Diffraction, 2006)'

_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.41340
_diffrn_radiation_type            synchrotron
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Oxford Xcalibur 3'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          11
_diffrn_standards_interval_count  160
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             651
_diffrn_reflns_av_R_equivalents   0.1252
_diffrn_reflns_av_sigmaI/netI     0.0845
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -5
_diffrn_reflns_limit_l_max        5
_diffrn_reflns_theta_min          1.57
_diffrn_reflns_theta_max          13.28
_reflns_number_total              411
_reflns_number_gt                 373
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Crysalis (Oxford Diffraction, 2006)'
_computing_cell_refinement        'Crysalis (Oxford Diffraction, 2006)'
_computing_data_reduction         'Crysalis (Oxford Diffraction, 2006)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     'Xtaldraw (Downs & Hall-Wallace, 2003)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 2008)'
 
_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)+(0.0356P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_refine_ls_hydrogen_treatment     none
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          411
_refine_ls_number_parameters      73
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0383
_refine_ls_R_factor_gt            0.0372
_refine_ls_wR_factor_ref          0.0868
_refine_ls_wR_factor_gt           0.0866
_refine_ls_goodness_of_fit_ref    1.374
_refine_ls_restrained_S_all       1.374
_refine_ls_shift/su_max           0.000
_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
Ca Ca 0.00001(2) 0.17120(3) 0.25001(3) 0.0398(5) Uani 1 1 d . . .
S S 0.00000(3) 0.31962(4) 0.74989(4) 0.0401(5) Uani 1 1 d . . .
O1A O 0.0831(2) 0.26517(7) 0.5892(3) 0.0386(5) Uani 1 1 d . . .
O1B O 0.5961(2) 0.77173(7) 0.5914(3) 0.0387(5) Uani 1 1 d . . .
O2A O 0.1965(2) 0.38053(6) 0.9016(4) 0.0389(6) Uani 1 1 d . . .
O2B O 0.6897(2) 0.88058(6) 0.9085(4) 0.0391(6) Uani 1 1 d . . .
OWA O -0.1900(2) 0.06393(6) -0.0770(4) 0.0409(5) Uani 1 1 d . . .
OWB O 0.3100(2) 0.55847(7) -0.0755(4) 0.0416(5) Uani 1 1 d . . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Ca 0.0457(8) 0.0326(5) 0.0433(11) 0.00003(4) 0.0211(8) 0.00019(4)
S 0.0457(8) 0.0334(6) 0.0436(12) -0.00015(5) 0.0214(8) -0.00020(5)
O1A 0.0457(8) 0.0264(6) 0.0453(12) 0.0001(4) 0.0209(9) -0.0006(4)
O1B 0.0457(8) 0.0263(6) 0.0458(12) -0.0001(5) 0.0212(8) -0.0010(4)
O2A 0.0466(10) 0.0286(7) 0.0442(16) -0.0002(5) 0.0219(11) -0.0003(4)
O2B 0.0460(10) 0.0295(7) 0.0442(15) -0.0001(5) 0.0216(11) -0.0004(4)
OWA 0.0461(9) 0.0348(7) 0.0426(12) -0.0001(6) 0.0198(9) 0.0001(4)
OWB 0.0464(9) 0.0366(6) 0.0427(12) -0.0006(6) 0.0200(9) 0.0008(4)
 
_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
Ca O1A 2.217(4) . ?
Ca O1B 2.281(4) 2_545 ?
Ca O1B 2.312(5) 3_666 ?
Ca OWA 2.313(4) . ?
Ca OWB 2.366(4) 2_545 ?
Ca O2A 2.393(4) 4_565 ?
Ca O1A 2.415(5) 4_565 ?
Ca O2B 2.454(4) 3_666 ?
Ca S 2.936(6) 4_565 ?
Ca S 2.936(6) 4_665 ?
Ca Ca 3.855(8) 4_666 ?
Ca Ca 3.855(8) 4_565 ?
S O2B 1.417(3) 2_546 ?
S O1B 1.418(2) 2_546 ?
S O2A 1.428(3) . ?
S O1A 1.432(2) . ?
S Ca 2.936(6) 4_666 ?
S Ca 2.936(6) 4_566 ?
O1A Ca 2.415(5) 4_666 ?
O1B S 1.418(2) 2_556 ?
O1B Ca 2.281(4) 2 ?
O1B Ca 2.312(5) 3_666 ?
O2A Ca 2.393(4) 4_666 ?
O2B S 1.417(3) 2_556 ?
O2B Ca 2.454(4) 3_666 ?
OWB Ca 2.366(4) 2 ?
 
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
O1A Ca O1B 98.81(17) . 2_545 ?
O1A Ca O1B 67.99(16) . 3_666 ?
O1B Ca O1B 85.20(19) 2_545 3_666 ?
O1A Ca OWA 162.70(6) . . ?
O1B Ca OWA 87.66(18) 2_545 . ?
O1B Ca OWA 128.85(12) 3_666 . ?
O1A Ca OWB 87.79(17) . 2_545 ?
O1B Ca OWB 164.79(6) 2_545 2_545 ?
O1B Ca OWB 84.61(18) 3_666 2_545 ?
OWA Ca OWB 89.96(19) . 2_545 ?
O1A Ca O2A 81.16(15) . 4_565 ?
O1B Ca O2A 122.70(14) 2_545 4_565 ?
O1B Ca O2A 141.73(13) 3_666 4_565 ?
OWA Ca O2A 81.85(15) . 4_565 ?
OWB Ca O2A 71.71(15) 2_545 4_565 ?
O1A Ca O1A 83.03(19) . 4_565 ?
O1B Ca O1A 65.23(15) 2_545 4_565 ?
O1B Ca O1A 134.84(12) 3_666 4_565 ?
OWA Ca O1A 85.21(18) . 4_565 ?
OWB Ca O1A 129.53(12) 2_545 4_565 ?
O2A Ca O1A 57.86(13) 4_565 4_565 ?
O1A Ca O2B 124.64(14) . 3_666 ?
O1B Ca O2B 83.17(14) 2_545 3_666 ?
O1B Ca O2B 56.99(13) 3_666 3_666 ?
OWA Ca O2B 71.88(15) . 3_666 ?
OWB Ca O2B 81.81(14) 2_545 3_666 ?
O2A Ca O2B 142.51(9) 4_565 3_666 ?
O1A Ca O2B 141.73(13) 4_565 3_666 ?
O1A Ca S 80.33(17) . 4_565 ?
O1B Ca S 94.12(16) 2_545 4_565 ?
O1B Ca S 147.75(8) 3_666 4_565 ?
OWA Ca S 83.23(16) . 4_565 ?
OWB Ca S 100.52(15) 2_545 4_565 ?
O2A Ca S 28.86(7) 4_565 4_565 ?
O1A Ca S 29.01(8) 4_565 4_565 ?
O2B Ca S 155.03(7) 3_666 4_565 ?
O1A Ca S 96.22(17) . 4_665 ?
O1B Ca S 82.27(16) 2_545 4_665 ?
O1B Ca S 28.29(8) 3_666 4_665 ?
OWA Ca S 100.56(15) . 4_665 ?
OWB Ca S 83.40(15) 2_545 4_665 ?
O2A Ca S 155.03(7) 4_565 4_665 ?
O1A Ca S 146.83(8) 4_565 4_665 ?
O2B Ca S 28.74(7) 3_666 4_665 ?
S Ca S 174.61(3) 4_565 4_665 ?
O1A Ca Ca 35.33(9) . 4_666 ?
O1B Ca Ca 91.21(18) 2_545 4_666 ?
O1B Ca Ca 32.68(9) 3_666 4_666 ?
OWA Ca Ca 161.44(5) . 4_666 ?
OWB Ca Ca 86.28(19) 2_545 4_666 ?
O2A Ca Ca 113.98(15) 4_565 4_666 ?
O1A Ca Ca 111.08(16) 4_565 4_666 ?
O2B Ca Ca 89.59(15) 3_666 4_666 ?
S Ca Ca 115.33(14) 4_565 4_666 ?
S Ca Ca 60.96(14) 4_665 4_666 ?
O1A Ca Ca 91.79(18) . 4_565 ?
O1B Ca Ca 33.18(9) 2_545 4_565 ?
O1B Ca Ca 112.63(16) 3_666 4_565 ?
OWA Ca Ca 84.86(19) . 4_565 ?
OWB Ca Ca 161.19(5) 2_545 4_565 ?
O2A Ca Ca 89.64(15) 4_565 4_565 ?
O1A Ca Ca 32.07(9) 4_565 4_565 ?
O2B Ca Ca 113.44(15) 3_666 4_565 ?
S Ca Ca 60.94(14) 4_565 4_565 ?
S Ca Ca 115.31(14) 4_665 4_565 ?
Ca Ca Ca 104.08(18) 4_666 4_565 ?
O2B S O1B 106.88(15) 2_546 2_546 ?
O2B S O2A 99.7(2) 2_546 . ?
O1B S O2A 113.74(17) 2_546 . ?
O2B S O1A 112.23(17) 2_546 . ?
O1B S O1A 114.53(15) 2_546 . ?
O2A S O1A 108.83(15) . . ?
O2B S Ca 119.52(14) 2_546 4_666 ?
O1B S Ca 133.04(13) 2_546 4_666 ?
O2A S Ca 53.99(12) . 4_666 ?
O1A S Ca 54.87(13) . 4_666 ?
O2B S Ca 56.40(13) 2_546 4_566 ?
O1B S Ca 50.58(13) 2_546 4_566 ?
O2A S Ca 121.82(13) . 4_566 ?
O1A S Ca 129.01(13) . 4_566 ?
Ca S Ca 174.61(3) 4_666 4_566 ?
S O1A Ca 150.40(12) . . ?
S O1A Ca 96.12(15) . 4_666 ?
Ca O1A Ca 112.60(15) . 4_666 ?
S O1B Ca 144.66(12) 2_556 2 ?
S O1B Ca 101.12(16) 2_556 3_666 ?
Ca O1B Ca 114.14(15) 2 3_666 ?
S O2A Ca 97.14(15) . 4_666 ?
S O2B Ca 94.86(16) 2_556 3_666 ?
 
_diffrn_measured_fraction_theta_max    0.657
_diffrn_reflns_theta_full              13.28
_diffrn_measured_fraction_theta_full   0.657
_refine_diff_density_max    0.433
_refine_diff_density_min   -0.387
_refine_diff_density_rms    0.131
