Mixed-valence dimolybdenum complexes containing hard oxo and soft carbonyl ligands: synthesis, structure, and electrochemistry of Mo<sub>2</sub>(O)(CO)<sub>2</sub>(μ-κ<sup>2</sup>-S(CH<sub>2</sub>)<sub>n</sub>S)<sub>2</sub>(κ<sup>2</sup>-diphosphine).
Haque, Mohd Rezaul; Ghosh, Shishir; Rahman, Md Matiar; Siddiquee, Tasneem A.; Nesterov, Vladimir N.; Richmond, Michael G.; Hogarth, Graeme; Kabir, Shariff E.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10102–10112; doi:10.1039/c8dt02231c

data_7046896
_publ_section_title
;
 Mixed-valence dimolybdenum complexes containing hard oxo and soft
 carbonyl ligands: synthesis, structure, and electrochemistry of
 Mo<sub>2</sub>(O)(CO)<sub>2</sub>(\m-\k<sup>2</sup>-S(CH<sub>2</sub>)<sub>n</sub>S)<sub>2</sub>(\k<sup>2</sup>-diphosphine).
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10102
_journal_page_last               10112
_journal_paper_doi               10.1039/c8dt02231c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C33 H34 Mo2 O3 P2 S4'
_chemical_formula_sum            'C33 H34 Mo2 O3 P2 S4'
_chemical_formula_weight         860.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-19 deposited with the CCDC.
2018-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.143(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.152(3)
_cell_length_b                   15.879(3)
_cell_length_c                   18.565(4)
_cell_measurement_reflns_used    8187
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      3.04
_cell_volume                     3582.3(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury375R/M CCD (XtaLAB mini)'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1148
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26643
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.042
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.8703
_exptl_transmission_factor_min   0.3457
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.4262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4530
_reflns_number_total             7292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02231c2.cif
_cod_data_source_block           sid047new
_cod_depositor_comments
'Adding full bibliography for 7046894--7046896.cif.'
_cod_original_cell_volume        3582.2(13)
_cod_database_code               7046896
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.801
_exptl_absorpt_special_details   SADABS
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
;
_olex2_submission_special_instructions 'No special instructions were received'