A 3:1 Disordered Solid Solution of Di-μ-methoxo-<i>O</i>:<i>O</i>-bis[trimethoxooxomolybdenum(VI)] and Di-μ-methoxo-<i>O</i>:<i>O</i>-bis[chlorodimethoxooxomolybdenum(VI)]
Clegg, W.; Elsegood, M. R. J.; Errington, R. J.; Bakri, R.; Acta Crystallographica Section C 52 (1996) 2145–2148; doi:10.1107/S0108270196006257

data_2005362
_publ_section_title
;
 A 3:1 Disordered Solid Solution of
 Di-\m-methoxo-<i>O</i>:<i>O</i>-bis[trimethoxooxomolybdenum(VI)] and
 Di-\m-methoxo-<i>O</i>:<i>O</i>-bis[chlorodimethoxooxomolybdenum(VI)]
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2145
_journal_page_last               2148
_journal_paper_doi               10.1107/S0108270196006257
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety
'(C8 H24 Mo2 O10)0.75, (C6 H18 Cl2 Mo2 O8)0.25'
_chemical_formula_sum            'C7.5 H22.5 Cl0.5 Mo2 O9.5'
_chemical_formula_weight         474.36
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.
_cell_angle_beta                 92.38(7)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   11.798(3)
_cell_length_b                   10.259(3)
_cell_length_c                   13.326(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      10.57
_cell_volume                     1611.5(8)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device
'Stoe-Siemens diffractometer with Cryostream cooler (Cosier & Glazer, 1986)'
_diffrn_measurement_method
'\w/\q scans with on-line profile fitting (Clegg, 1981)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4826
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.675
_exptl_absorpt_correction_T_max  0.295
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   'empirical from \y scans (Sheldrick, 1994)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.615
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_all   1.122
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_hydrogen_treatment    'H atoms riding, C-H 0.98\%A'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_obs          0.0303
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0207P)^2^ + 4.4949P]
where P = (F~o~^2^ + 2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.0783
_refine_ls_wR_factor_obs         0.0710
_reflns_number_observed          2279
_reflns_number_total             2711
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            fg1191.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2005362