Preparation of a bis(hydrosulfido) complex of Mo having a tetraphosphine co-ligand and its transformation into MoRh2 and MoIr2 mixed-metal sulfido clusters
Iwasa, Kentaro; Seino, Hidetake; Niikura, Fumiya; Mizobe, Yasushi; Dalton Transactions  (2009) 6134–; doi:10.1039/b902386k

data_7001767
_publ_section_title
;
 Preparation of a bis(hydrosulfido) complex of Mo having a
 tetraphosphine co-ligand and its transformation into MoRh2 and MoIr2
 mixed-metal sulfido clusters
;
_journal_issue                   31
_journal_name_full               'Dalton Transactions'
_journal_page_first              6134
_journal_paper_doi               10.1039/b902386k
_journal_year                    2009
_chemical_formula_moiety         'C50 H42 Mo O4 P4 Rh2 S2, 1.3(C H2 Cl2)'
_chemical_formula_sum            'C51.3 H44.6 Cl2.6 Mo O4 P4 Rh2 S2'
_chemical_formula_weight         1307.06
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.1025(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   41.2344(14)
_cell_length_b                   11.9799(4)
_cell_length_c                   21.7291(9)
_cell_measurement_reflns_used    13829
_cell_measurement_temperature    293.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     10673.0(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41536
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5220.80
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.47
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     638
_refine_ls_number_reflns         12020
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 0.6000\s(Fo^2^) + 0.1500]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                8735
_reflns_number_total             12020
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b902386k.txt
_cod_data_source_block           '__[Mo(P4)(mu3-S)2{Rh(CO)2}2]-1.3(CH2Cl2)_(4a)'
_cod_original_formula_sum        'C51.30 H44.60 Cl2.60 Mo O4 P4 Rh2 S2 '
_cod_database_code               7001767