Tetrakis(benzyldiphenylphosphine-κ<i>P</i>)tetra-μ~2~-sulfido-dicopper(I)molybdenum(VI) tetrahydrate
Niu, Yun-Yin; Shui, You-Qin; Yang, Rui; Ng, Seik Weng; Acta Crystallographica Section E 62 (2006) m939–m941; doi:10.1107/S1600536806011111

data_2208936
_publ_section_title
;Tetrakis(benzyldiphenylphosphine-\k<i>P</i>)tetra-\m~2~-sulfido-dicopper(I)molybdenum(VI)
 tetrahydrate
;
_journal_coeditor_code           LH2030
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m939
_journal_page_last               m941
_journal_paper_doi               10.1107/S1600536806011111
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mo Cu2 S4 (C19 H17 P)4], 4H2 O'
_chemical_formula_moiety         'C76 H68 Cu2 Mo P4 S4, 4H2 O'
_chemical_formula_sum            'C76 H76 Cu2 Mo O4 P4 S4'
_chemical_formula_weight         1528.51
_chemical_name_systematic
;
Tetrakis(benzyldiphenylphosphine-\kP)tetra-\m~2~-sulfido-
dicopper(I)molybdenum(VI) tetrahydrate
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7770(10)
_cell_length_b                   13.777
_cell_length_c                   22.995(2)
_cell_measurement_reflns_used    3407
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      2.7
_cell_volume                     4364.6(5)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Bruker APEX-II area-detector'
_diffrn_measurement_method       '\f and \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  0.017
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9215
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.7
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details 'Flack (1983), 2328 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4886
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0923P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                3959
_reflns_number_total             4886
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2030.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-21

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4364.3(4)
_cod_database_code               2208936
_cod_database_fobs_code          2208936