μ-Oxo-bis[dichlorooxo(trimethylphosphine-<i>P</i>)(trimethylphosphine oxide-<i>O</i>)molybdenum(V)] diethyl ether hemisolvate
Cotton, F. Albert; Daniels, Lee M.; Herrero, Santiago; Acta Crystallographica Section C 55 (1999) IUC9900018–; doi:10.1107/S010827019909976X

data_2008290
_publ_section_title
;
 \m-Oxo-bis[dichlorooxo(trimethylphosphine-<i>P</i>)(trimethylphosphine
 oxide-<i>O</i>)molybdenum(V)] diethyl ether hemisolvate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900018
_journal_paper_doi               10.1107/S010827019909976X
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac
'[Mo2 Cl4 O3 (C3 H9 P1)2 (C3 H9 O1 P1)2], 0.5C4 H10 O'
_chemical_formula_moiety         'C12 H36 Cl4 Mo2 O5 P4, 0.5C4 H10 O'
_chemical_formula_sum            'C14 H41 Cl4 Mo2 O5.5 P4'
_chemical_formula_weight         755.03
_chemical_name_systematic
;
\m-oxobis[(trimethylphosphine-P)(trimethylphosphine oxide-O)dichloro-
oxomolybdenum(V)] diethylether semisolvate
;
_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                90.00
_cell_angle_beta                 104.960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.263(2)
_cell_length_b                   11.285(2)
_cell_length_c                   30.361(5)
_cell_measurement_reflns_used    247
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.9
_cell_volume                     6376.3(17)
_computing_cell_refinement       'MADNES (Pflugrath & Messerschmidt, 1992)'
_computing_data_collection       'MADNES (Pflugrath & Messerschmidt, 1992)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1996)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST'
_diffrn_measurement_method       \w
_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  0.053
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            30841
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.874
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.203
_refine_ls_goodness_of_fit_obs   1.137
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         11168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.237
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.093
_refine_ls_R_factor_obs          0.062
_refine_ls_shift/esd_max         <0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0001P)^2^+81.9606P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.147
_refine_ls_wR_factor_obs         0.117
_reflns_number_observed          8599
_reflns_number_total             11229
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            qb0081.cif
_cod_data_source_block           QB0081
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0001P)^2^+81.9606P] where P = (Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0001P)^2^+81.9606P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C14 H41 Cl4 Mo2 O5.50 P4'
_cod_database_code               2008290