"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_4116937
_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            'C40 H99 Mg Mo2 N12 O2.5 Si6'
_chemical_formula_weight         1171.04
_chemical_name_systematic
; 
 ? 
;
_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                89.4350(10)
_cell_angle_beta                 84.1230(10)
_cell_angle_gamma                82.19
_cell_formula_units_Z            2
_cell_length_a                   10.1540(2)
_cell_length_b                   16.4300(3)
_cell_length_c                   19.8388(5)
_cell_measurement_temperature    183(2)
_cell_volume                     3261.75(12)
_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  0.1638
_diffrn_reflns_av_sigmaI/netI    0.1164
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9883
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.8745
_exptl_absorpt_correction_T_min  0.3810
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             1245
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.0007(6)
_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   1.165
_refine_ls_goodness_of_fit_obs   1.195
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         5892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_restrained_S_obs      1.195
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_obs          0.0907
_refine_ls_shift/esd_max         0.164
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+36.3271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2435
_refine_ls_wR_factor_obs         0.2274
_reflns_number_observed          5422
_reflns_number_total             6054
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja963822y_1.cif
_cod_data_source_block           C40H99MgMo2N12O2.50Si6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+36.3271P] 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^)+(0.0707P)^2^+36.3271P] 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        3261.77(12)
_cod_original_formula_sum        'C40 H99 Mg Mo2 N12 O2.50 Si6'
_cod_database_code               4116937