Four-Coordinate Molybdenum Chalcogenide Complexes Relevant to Nitrous Oxide N-N Bond Cleavage by Three-Coordinate Molybdenum(III): Synthesis, Characterization, Reactivity, and Thermochemistry
Adam R. Johnson; William M. Davis; Christopher C. Cummins; Scafford Serron; Steven P. Nolan; Djamaladdin G. Musaev; Keiji Morokuma; Journal of the American Chemical Society 120 (1998) 2071–2085; doi:10.1021/ja971491z

data_4116701
_publ_contact_author
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    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
;
 Four-Coordinate Molybdenum Chalcogenide Complexes Relevant to Nitrous
 Oxide N-N Bond Cleavage by Three-Coordinate Molybdenum(III): Synthesis,
 Characterization, Reactivity, and Thermochemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2071
_journal_page_last               2085
_journal_paper_doi               10.1021/ja971491z
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C81 H119 Mo2 N6 O2 S'
_chemical_formula_weight         1432.76
_chemical_name_systematic
'carbonsulfide(tris(N-tert-butylanilido)molybdenum dimer'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                81.1990(10)
_cell_angle_beta                 77.8370(10)
_cell_angle_gamma                67.6530(10)
_cell_formula_units_Z            2
_cell_length_a                   14.6441(3)
_cell_length_b                   15.2700(2)
_cell_length_c                   20.5956(4)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      1.45
_cell_volume                     4150.44(13)
_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      153(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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11885
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.4673
_exptl_absorpt_correction_T_min  0.3968
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       needles
_exptl_crystal_F_000             1526
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.209
_refine_ls_goodness_of_fit_obs   1.268
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         7484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.470
_refine_ls_restrained_S_obs      1.268
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_obs          0.1035
_refine_ls_shift/esd_max         -0.858
_refine_ls_shift/esd_mean        0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+72.9610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2697
_refine_ls_wR_factor_obs         0.2107
_reflns_number_observed          6252
_reflns_number_total             7493
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja971491z_5.cif
_cod_data_source_block           s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+72.9610P] 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^)+(0.0001P)^2^+72.9610P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4116701