In Pursuit of the Molybdenum(III) Tris(thiolate) Fragment: Unusual Structure of a Dimolybdenum μ-Nitrido Complex
Theodor Agapie; Aaron L. Odom; Christopher C. Cummins; Inorganic Chemistry 39 (2000) 174–179; doi:10.1021/ic9904891

data_4300033
_publ_contact_author
;
    Christopher C. Cummins
    Massachusetts Institute of Technology
    Department of Chemistry
    77 Massachusetts Ave.
    Cambridge, MA 02139
    USA
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_fax         '(1) 617 253 7030'
_publ_contact_author_phone       '(1) 617 253 5332'
_publ_section_title
;
In Pursuit of the Molybdenum(III) Tris(thiolate) Fragment: Unusual
Structure of a Dimolybdenum \m-Nitrido Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              174
_journal_page_last               179
_journal_paper_doi               10.1021/ic9904891
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C60 H87 Mo2 N4 S3'
_chemical_formula_weight         1152.39
_chemical_name_systematic
; 
 (mu)-nitrido tris-thioadamantyl tris-(N-tert-butyl anilido) 
dimolybdenum(IV, V)
;
_space_group_IT_number           147
_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.677(3)
_cell_length_b                   15.677(3)
_cell_length_c                   16.021(2)
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      1.50
_cell_volume                     3409.9(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13428
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.9141
_exptl_absorpt_correction_T_min  0.8358
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       plate
_exptl_crystal_F_000             1214
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.896
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.0021(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.110
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_obs          0.0588
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+12.4443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2110
_refine_ls_wR_factor_obs         0.1823
_reflns_number_observed          2850
_reflns_number_total             3261
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+12.4443P] 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^)+(0.1149P)^2^+12.4443P] where P=(Fo^2^+2Fc^2^)/3'.

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

2021-10-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H58 Mo1.33 N2.67 S2'
_cod_original_formula_weight         768.26
_cod_original_formula_units_Z            3
_cod_original_cell_volume        3410.1(9)
_cod_database_code               4300033