X-ray Structure of (Bun4N)[Mo(1,2-Benzenedithiolate)3]. Trigonal-Prismatic versus Octahedral Coordination in Tris(1,2-Benzenedithiolate) Complexes
Antonio Cervilla; Elisa Llopis; Dolores Marco; Francisco Pérez; Inorganic Chemistry 40 (2001) 6525–6528; doi:10.1021/ic010327g

data_4320627
_publ_section_title
;
 X-ray Structure of (Bun4N)[Mo(1,2-Benzenedithiolate)3].
 Trigonal-Prismatic versus Octahedral Coordination in
 Tris(1,2-Benzenedithiolate) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6525
_journal_page_last               6528
_journal_paper_doi               10.1021/ic010327g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C34 H48 Mo N S6'
_chemical_formula_weight         758.75
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.749(4)
_cell_length_b                   11.019(3)
_cell_length_c                   17.324(5)
_cell_measurement_temperature    298(2)
_cell_volume                     3769.9(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2835
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2555
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.701
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_F_000             1444
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.379
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         2554
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.228
_refine_ls_R_factor_all          0.2813
_refine_ls_R_factor_obs          0.0863
_refine_ls_shift/esd_max         -0.039
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0740
_refine_ls_wR_factor_obs         0.0469
_reflns_number_observed          883
_reflns_number_total             2555
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010327g.cif
_cod_data_source_block           final
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2020-11-05
Z value fixed to be consistent with given formula
                 miguel
;
_cod_original_formula_units_Z            2
_cod_original_cell_volume        3770.0(16)
_cod_database_code               4320627