"Fixation" of Dinitrogen by Molybdenum and the Formation of a Trigonal Planar Iron-Tris[molybdenum(dinitrogen)] Complex
Myra B. O'Donoghue; Nadia C. Zanetti; William M. Davis; Richard R. Schrock; Journal of the American Chemical Society 119 (1997) 2753–2754; doi:10.1021/ja963822y

data_4116939
_publ_section_title
;
 "Fixation" of Dinitrogen by Molybdenum and the Formation of a Trigonal
 Planar Iron-Tris[molybdenum(dinitrogen)] Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2753
_journal_page_last               2754
_journal_paper_doi               10.1021/ja963822y
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C15 H39 Mo N6 Si3'
_chemical_formula_weight         483.73
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            16
_cell_length_a                   17.0164(2)
_cell_length_b                   16.9922(3)
_cell_length_c                   34.251
_cell_measurement_temperature    183(2)
_cell_volume                     9903.5(2)
_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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            30723
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00006(2)
_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   1.245
_refine_ls_goodness_of_fit_obs   1.269
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.300
_refine_ls_restrained_S_obs      1.269
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_obs          0.0459
_refine_ls_shift/esd_max         0.024
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+23.9345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1060
_refine_ls_wR_factor_obs         0.0969
_reflns_number_observed          6261
_reflns_number_total             7087
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja963822y_3.cif
_cod_data_source_block           C15H39MoN6Si3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+23.9345P] 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^)+(0.0217P)^2^+23.9345P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9903.7(2)
_cod_database_code               4116939