 
data_blue-crystal
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             'gelosaite (Su Senargiu)'
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Bi H3 Mo2.19 O9'
_chemical_formula_weight          566.11
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mo'  'Mo'  -1.6832   0.6857
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Bi'  'Bi'  -4.1077  10.2566
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/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                    5.8570(5)
_cell_length_b                    9.0517(8)
_cell_length_c                    13.9923(12)
_cell_angle_alpha                 90.00
_cell_angle_beta                  100.44(1)
_cell_angle_gamma                 90.00
_cell_volume                      729.53(11)
_cell_formula_units_Z             4
_cell_measurement_temperature     292(2)
_cell_measurement_reflns_used     4232
_cell_measurement_theta_min       2.70
_cell_measurement_theta_max       30.73
 
_exptl_crystal_description        prism
_exptl_crystal_colour             pale-blue
_exptl_crystal_size_max           0.06
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     5.127
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              999.9
_exptl_absorpt_coefficient_mu     27.78
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.544
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    SADABS
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       292(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   'APEX II CCD diffractometer'
_diffrn_measurement_method        'omega scan'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             10605
_diffrn_reflns_av_R_equivalents   0.0659
_diffrn_reflns_av_sigmaI/netI     0.0474
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          2.69
_diffrn_reflns_theta_max          31.22
_reflns_number_total              2233
_reflns_number_gt                 1661
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_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)+(0.0658P)²+10.3301P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    ?
_refine_ls_hydrogen_treatment     none
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          2233
_refine_ls_number_parameters      119
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0628
_refine_ls_R_factor_gt            0.0439
_refine_ls_wR_factor_ref          0.1216
_refine_ls_wR_factor_gt           0.1109
_refine_ls_goodness_of_fit_ref    1.063
_refine_ls_restrained_S_all       1.063
_refine_ls_shift/su_max           0.017
_refine_ls_shift/su_mean          0.018
 
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
Bi Bi 0.40429(2) 0.416795(15) 0.106446(9) 0.00984(3) Uani 1 1 d . . .
Mo1 Mo 0.86595(5) 0.10354(3) 0.15724(2) 0.00785(7) Uani 1 1 d . . .
Mo2 Mo 0.63243(5) 0.22196(3) 0.34088(2) 0.00912(7) Uani 1 1 d . . .
Mo3 Mo 0.6321(9) -0.0434(6) 0.3426(4) 0.0054(9) Uiso 0.06 1 d P . .
Mo4 Mo 1.0950(4) 0.2626(3) 0.39300(16) 0.0087(4) Uiso 0.13 1 d P . .
OW O 0.9599(5) 0.4184(4) 0.3433(2) 0.0208(7) Uani 1 1 d . . .
O2 O 0.7548(5) 0.0937(3) 0.0332(2) 0.0164(7) Uani 1 1 d . . .
O3 O 0.3995(5) 0.1067(3) 0.3362(2) 0.0182(7) Uani 1 1 d . . .
O4 O 0.6401(4) 0.2407(3) 0.19042(17) 0.0126(6) Uani 1 1 d . . .
O5 O 0.7469(5) 0.2440(4) 0.46441(17) 0.0167(6) Uani 1 1 d . . .
OH O 0.8232(5) -0.0893(3) 0.48088(18) 0.0136(6) Uani 1 1 d . . .
O7 O 1.0129(4) -0.0878(3) 0.18297(19) 0.0106(6) Uani 1 1 d . . .
O8 O 0.8659(4) 0.0858(3) 0.31166(17) 0.0099(6) Uani 1 1 d . . .
O9 O 1.1005(5) 0.2166(3) 0.1645(2) 0.0201(8) Uani 1 1 d . . .
 
 
_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
Bi OH 2.180(3) 2_655 ?
Bi O8 2.215(3) 2_655 ?
Bi O4 2.289(3) . ?
Bi OH 2.334(3) 4_565 ?
Bi O5 2.501(3) 4_565 ?
Bi O3 2.699(3) 2 ?
Bi Mo3 2.704(5) 2_655 ?
Bi Mo4 3.130(3) 2_655 ?
Bi Mo3 3.364(5) 2 ?
Bi Bi 3.6891(16) 3_665 ?
Mo1 O9 1.701(3) . ?
Mo1 O2 1.742(3) . ?
Mo1 O4 1.931(3) . ?
Mo1 O7 1.938(3) . ?
Mo1 O8 2.167(2) . ?
Mo1 Mo3 3.196(5) 2_655 ?
Mo2 O3 1.709(3) . ?
Mo2 O5 1.748(3) . ?
Mo2 O7 1.923(3) 2_655 ?
Mo2 O8 1.939(3) . ?
Mo2 O4 2.121(2) . ?
Mo2 Mo3 2.402(5) . ?
Mo2 Mo4 2.700(3) . ?
Mo3 O8 1.909(6) . ?
Mo3 O3 1.915(6) . ?
Mo3 OH 2.094(6) . ?
Mo3 O4 2.457(6) 2_645 ?
Mo3 Bi 2.704(5) 2_645 ?
Mo3 Mo1 3.196(5) 2_645 ?
Mo3 Bi 3.364(5) 2_545 ?
Mo4 OW 1.703(4) . ?
Mo4 O8 2.259(4) . ?
Mo4 OH 2.345(4) 3_756 ?
Mo4 O2 2.398(4) 4_666 ?
Mo4 O5 2.434(4) . ?
Mo4 O3 2.513(4) 1_655 ?
Mo4 Bi 3.130(3) 2_645 ?
O2 Mo4 2.398(4) 4_565 ?
O3 Mo4 2.513(4) 1_455 ?
O3 Bi 2.699(3) 2_545 ?
O4 Mo3 2.457(6) 2_655 ?
O5 Bi 2.501(3) 4_666 ?
OH Bi 2.180(3) 2_645 ?
OH Bi 2.334(3) 4_666 ?
OH Mo4 2.345(4) 3_756 ?
O7 Mo2 1.923(3) 2_645 ?
O8 Bi 2.215(3) 2_645 ?
 
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
OH Bi O8 82.50(10) 2_655 2_655 ?
OH Bi O4 80.51(9) 2_655 . ?
O8 Bi O4 87.80(11) 2_655 . ?
OH Bi OH 70.42(12) 2_655 4_565 ?
O8 Bi OH 87.09(11) 2_655 4_565 ?
O4 Bi OH 150.89(10) . 4_565 ?
OH Bi O5 75.03(10) 2_655 4_565 ?
O8 Bi O5 156.21(10) 2_655 4_565 ?
O4 Bi O5 95.96(11) . 4_565 ?
OH Bi O5 78.22(10) 4_565 4_565 ?
OH Bi O3 140.54(10) 2_655 2 ?
O8 Bi O3 77.16(9) 2_655 2 ?
O4 Bi O3 131.29(9) . 2 ?
OH Bi O3 75.07(10) 4_565 2 ?
O5 Bi O3 116.05(10) 4_565 2 ?
OH Bi Mo3 49.37(13) 2_655 2_655 ?
O8 Bi Mo3 44.30(14) 2_655 2_655 ?
O4 Bi Mo3 58.24(14) . 2_655 ?
OH Bi Mo3 99.62(15) 4_565 2_655 ?
O5 Bi Mo3 119.68(15) 4_565 2_655 ?
O3 Bi Mo3 121.42(13) 2 2_655 ?
OH Bi Mo4 91.49(8) 2_655 2_655 ?
O8 Bi Mo4 46.19(8) 2_655 2_655 ?
O4 Bi Mo4 133.99(8) . 2_655 ?
OH Bi Mo4 48.15(8) 4_565 2_655 ?
O5 Bi Mo4 125.74(8) 4_565 2_655 ?
O3 Bi Mo4 50.42(8) 2 2_655 ?
Mo3 Bi Mo4 82.26(12) 2_655 2_655 ?
OH Bi Mo3 158.18(11) 2_655 2 ?
O8 Bi Mo3 108.64(12) 2_655 2 ?
O4 Bi Mo3 117.74(11) . 2 ?
OH Bi Mo3 91.00(13) 4_565 2 ?
O5 Bi Mo3 90.40(12) 4_565 2 ?
O3 Bi Mo3 34.66(11) 2 2 ?
Mo3 Bi Mo3 149.49(19) 2_655 2 ?
Mo4 Bi Mo3 83.87(10) 2_655 2 ?
OH Bi Bi 36.59(8) 2_655 3_665 ?
O8 Bi Bi 83.72(8) 2_655 3_665 ?
O4 Bi Bi 117.09(7) . 3_665 ?
OH Bi Bi 33.83(7) 4_565 3_665 ?
O5 Bi Bi 73.63(7) 4_565 3_665 ?
O3 Bi Bi 107.05(8) 2 3_665 ?
Mo3 Bi Bi 73.80(13) 2_655 3_665 ?
Mo4 Bi Bi 66.00(4) 2_655 3_665 ?
Mo3 Bi Bi 124.02(11) 2 3_665 ?
O9 Mo1 O2 104.04(16) . . ?
O9 Mo1 O4 100.34(13) . . ?
O2 Mo1 O4 97.11(13) . . ?
O9 Mo1 O7 101.53(13) . . ?
O2 Mo1 O7 102.28(13) . . ?
O4 Mo1 O7 146.12(12) . . ?
O9 Mo1 O8 97.51(14) . . ?
O2 Mo1 O8 157.25(12) . . ?
O4 Mo1 O8 71.59(12) . . ?
O7 Mo1 O8 80.14(12) . . ?
O9 Mo1 Mo3 52.81(14) . 2_655 ?
O2 Mo1 Mo3 93.01(13) . 2_655 ?
O4 Mo1 Mo3 50.16(13) . 2_655 ?
O7 Mo1 Mo3 153.11(11) . 2_655 ?
O8 Mo1 Mo3 94.25(12) . 2_655 ?
O3 Mo2 O5 105.55(16) . . ?
O3 Mo2 O7 102.40(13) . 2_655 ?
O5 Mo2 O7 98.48(14) . 2_655 ?
O3 Mo2 O8 101.10(13) . . ?
O5 Mo2 O8 97.03(14) . . ?
O7 Mo2 O8 147.10(12) 2_655 . ?
O3 Mo2 O4 99.85(15) . . ?
O5 Mo2 O4 154.02(12) . . ?
O7 Mo2 O4 81.05(12) 2_655 . ?
O8 Mo2 O4 72.48(12) . . ?
O3 Mo2 Mo3 52.27(16) . . ?
O5 Mo2 Mo3 96.05(16) . . ?
O7 Mo2 Mo3 153.64(14) 2_655 . ?
O8 Mo2 Mo3 50.82(15) . . ?
O4 Mo2 Mo3 95.17(15) . . ?
O3 Mo2 Mo4 148.04(11) . . ?
O5 Mo2 Mo4 62.05(14) . . ?
O7 Mo2 Mo4 108.40(10) 2_655 . ?
O8 Mo2 Mo4 55.40(9) . . ?
O4 Mo2 Mo4 93.24(13) . . ?
Mo3 Mo2 Mo4 97.83(13) . . ?
O8 Mo3 O3 95.1(3) . . ?
O8 Mo3 OH 92.6(2) . . ?
O3 Mo3 OH 116.1(3) . . ?
O8 Mo3 Mo2 51.94(15) . . ?
O3 Mo3 Mo2 44.91(14) . . ?
OH Mo3 Mo2 101.9(2) . . ?
O8 Mo3 O4 90.5(2) . 2_645 ?
O3 Mo3 O4 164.1(3) . 2_645 ?
OH Mo3 O4 78.36(19) . 2_645 ?
Mo2 Mo3 O4 142.4(2) . 2_645 ?
O8 Mo3 Bi 54.12(14) . 2_645 ?
O3 Mo3 Bi 141.2(3) . 2_645 ?
OH Mo3 Bi 52.17(15) . 2_645 ?
Mo2 Mo3 Bi 97.66(17) . 2_645 ?
O4 Mo3 Bi 52.40(12) 2_645 2_645 ?
O8 Mo3 Mo1 127.6(2) . 2_645 ?
O3 Mo3 Mo1 135.4(2) . 2_645 ?
OH Mo3 Mo1 78.43(17) . 2_645 ?
Mo2 Mo3 Mo1 179.4(2) . 2_645 ?
O4 Mo3 Mo1 37.13(10) 2_645 2_645 ?
Bi Mo3 Mo1 82.14(13) 2_645 2_645 ?
O8 Mo3 Bi 148.2(2) . 2_545 ?
O3 Mo3 Bi 53.28(15) . 2_545 ?
OH Mo3 Bi 98.4(2) . 2_545 ?
Mo2 Mo3 Bi 96.42(16) . 2_545 ?
O4 Mo3 Bi 120.96(19) 2_645 2_545 ?
Bi Mo3 Bi 149.49(19) 2_645 2_545 ?
Mo1 Mo3 Bi 84.04(12) 2_645 2_545 ?
OW Mo4 O8 101.02(16) . . ?
OW Mo4 OH 151.41(19) . 3_756 ?
O8 Mo4 OH 85.81(14) . 3_756 ?
OW Mo4 O2 88.21(17) . 4_666 ?
O8 Mo4 O2 154.75(15) . 4_666 ?
OH Mo4 O2 75.58(12) 3_756 4_666 ?
OW Mo4 O5 82.13(16) . . ?
O8 Mo4 O5 72.10(12) . . ?
OH Mo4 O5 73.56(13) 3_756 . ?
O2 Mo4 O5 86.18(13) 4_666 . ?
OW Mo4 O3 129.75(18) . 1_655 ?
O8 Mo4 O3 80.43(12) . 1_655 ?
OH Mo4 O3 78.61(13) 3_756 1_655 ?
O2 Mo4 O3 111.66(14) 4_666 1_655 ?
O5 Mo4 O3 141.85(15) . 1_655 ?
OW Mo4 Mo2 68.48(13) . . ?
O8 Mo4 Mo2 44.94(9) . . ?
OH Mo4 Mo2 99.81(13) 3_756 . ?
O2 Mo4 Mo2 121.23(14) 4_666 . ?
O5 Mo4 Mo2 39.39(7) . . ?
O3 Mo4 Mo2 124.95(11) 1_655 . ?
OW Mo4 Bi 146.04(15) . 2_645 ?
O8 Mo4 Bi 45.02(8) . 2_645 ?
OH Mo4 Bi 47.87(8) 3_756 2_645 ?
O2 Mo4 Bi 122.70(11) 4_666 2_645 ?
O5 Mo4 Bi 86.03(11) . 2_645 ?
O3 Mo4 Bi 55.86(9) 1_655 2_645 ?
Mo2 Mo4 Bi 82.25(6) . 2_645 ?
Mo1 O2 Mo4 143.84(17) . 4_565 ?
Mo2 O3 Mo3 82.8(2) . . ?
Mo2 O3 Mo4 104.63(15) . 1_455 ?
Mo3 O3 Mo4 157.4(2) . 1_455 ?
Mo2 O3 Bi 160.40(15) . 2_545 ?
Mo3 O3 Bi 92.05(19) . 2_545 ?
Mo4 O3 Bi 73.73(10) 1_455 2_545 ?
Mo1 O4 Mo2 109.02(13) . . ?
Mo1 O4 Bi 134.43(12) . . ?
Mo2 O4 Bi 116.48(13) . . ?
Mo1 O4 Mo3 92.71(16) . 2_655 ?
Mo2 O4 Mo3 111.11(17) . 2_655 ?
Bi O4 Mo3 69.36(14) . 2_655 ?
Mo2 O5 Mo4 78.56(13) . . ?
Mo2 O5 Bi 137.66(17) . 4_666 ?
Mo4 O5 Bi 98.68(12) . 4_666 ?
Mo3 OH Bi 78.46(18) . 2_645 ?
Mo3 OH Bi 124.37(19) . 4_666 ?
Bi OH Bi 109.58(12) 2_645 4_666 ?
Mo3 OH Mo4 146.1(2) . 3_756 ?
Bi OH Mo4 111.61(13) 2_645 3_756 ?
Bi OH Mo4 83.98(11) 4_666 3_756 ?
Mo2 O7 Mo1 126.89(13) 2_645 . ?
Mo3 O8 Mo2 77.25(19) . . ?
Mo3 O8 Mo1 113.7(2) . . ?
Mo2 O8 Mo1 106.89(13) . . ?
Mo3 O8 Bi 81.58(18) . 2_645 ?
Mo2 O8 Bi 135.70(13) . 2_645 ?
Mo1 O8 Bi 117.22(13) . 2_645 ?
Mo3 O8 Mo4 134.8(2) . . ?
Mo2 O8 Mo4 79.66(11) . . ?
Mo1 O8 Mo4 110.02(14) . . ?
Bi O8 Mo4 88.79(12) 2_645 . ?
 
_diffrn_measured_fraction_theta_max    0.939
_diffrn_reflns_theta_full              31.22
_diffrn_measured_fraction_theta_full   0.939
_refine_diff_density_max    3.404
_refine_diff_density_min   -4.317
_refine_diff_density_rms    0.550
