Catalytic silylation of dinitrogen with a dicobalt complex.
Siedschlag, Randall B.; Bernales, Varinia; Vogiatzis, Konstantinos D.; Planas, Nora; Clouston, Laura J.; Bill, Eckhard; Gagliardi, Laura; Lu, Connie C.; Journal of the American Chemical Society 137 (2015) 4638–4641; doi:10.1021/jacs.5b01445

data_4129376
_publ_section_title
;
 Catalytic silylation of dinitrogen with a dicobalt complex.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4638
_journal_page_last               4641
_journal_paper_doi               10.1021/jacs.5b01445
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C39 H60 Co2 N4 P3'
_chemical_formula_sum            'C39 H60 Co2 N4 P3'
_chemical_formula_weight         795.68
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 97.2230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.600(2)
_cell_length_b                   14.0091(13)
_cell_length_c                   12.6805(12)
_cell_measurement_reflns_used    2987
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.086
_cell_measurement_theta_min      2.467
_cell_volume                     4335.3(7)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9837
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.8028
_exptl_absorpt_correction_T_min  0.8028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
Unmodelable electron density was removed using PLATON SQUEEZE.
;
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.435(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         9837
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                8155
_reflns_number_total             9837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b01445_si_001.cif
_cod_data_source_block           12155s_complex1
_cod_original_cell_volume        4335.2(7)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4129376