Synthesis and characterization of cyano and isocyano complexes of bis(dithiolato) molybdenum using Me3SiCN: a route to a cyanide-bridged multimer to a monomer
Bose, Moumita; Moula, Golam; Begum, Ameerunisha; Sarkar, Sabyasachi; New Journal of Chemistry 42 (2018) 5580–; doi:10.1039/C8NJ00246K

data_7057091
_publ_section_title
;
 Synthesis and characterization of cyano and isocyano complexes of
 bis(dithiolato) molybdenum using Me3SiCN: a route to a cyanide-bridged
 multimer to a monomer
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5580
_journal_paper_doi               10.1039/C8NJ00246K
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C27 H15 Mo N5 P S4, C8 H20 N, C H2 Cl2'
_chemical_formula_sum            'C36 H37 Cl2 Mo N6 P S4'
_chemical_formula_weight         879.77
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2ac -2n'
_symmetry_space_group_name_H-M   'P n 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-07-13 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3765(11)
_cell_length_b                   15.2044(12)
_cell_length_c                   19.5310(16)
_cell_measurement_temperature    100(2)
_cell_volume                     3972.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega scans'
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19980
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.289
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.34(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6242
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+10.7953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                5599
_reflns_number_total             6242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj00246k2.cif
_cod_data_source_block           16marbm
_cod_depositor_comments
'Adding full bibliography for 7057091--7057093.cif.'
_cod_original_sg_symbol_H-M      Pn21a
_cod_database_code               7057091