Dinitrogen Complexes Supported by Tris(phosphino)silyl Ligands
Matthew T. Whited; Neal P. Mankad; Yunho Lee; Paul F. Oblad; Jonas C. Peters; Inorganic Chemistry 48 (2009) 2507–2517; doi:10.1021/ic801855y

data_4301685
_publ_contact_author_address
;Department of Chemistry
Massachusetts Institute of Technology
Cambridge, MA 02139
USA
;
_publ_contact_author_email       jcpeters@mit.edu
_publ_contact_author_name        'Jonas C. Peters'
_publ_section_title
;
Dinitrogen Complexes Supported by Tris(phosphino)silyl Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2507
_journal_page_last               2517
_journal_paper_doi               10.1021/ic801855y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C38 H54 Co F6 O6 P3 S2 Si'
_chemical_formula_weight         964.86
_chemical_name_common            {[SiPiPr3]Co(OTf)}{OTf}
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8159(10)
_cell_length_b                   14.3316(13)
_cell_length_c                   28.152(3)
_cell_measurement_reflns_used    2921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.32
_cell_measurement_theta_min      2.36
_cell_volume                     4363.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1289
_diffrn_reflns_av_sigmaI/netI    0.1398
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21873
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         24.09
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         6036
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1195P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2174
_reflns_number_gt                3592
_reflns_number_total             6036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801855y_si_001_12.cif
_cod_data_source_block           mtw40
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4363.9(7)
_cod_database_code               4301685