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_4129377
_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 N6 P3, C18 H36 K N2 O6'
_chemical_formula_sum            'C57 H96 Co2 K N8 O6 P3'
_chemical_formula_weight         1239.33
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.5306(17)
_cell_length_b                   19.8037(15)
_cell_length_c                   31.964(3)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.2575
_cell_measurement_theta_min      2.243
_cell_volume                     13629(2)
_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  0.1118
_diffrn_reflns_av_sigmaI/netI    0.0993
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            83137
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.9362
_exptl_absorpt_correction_T_min  0.7758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Unmodelable electron density were removed using PLATON SQUEEZE.
A volume of 212 Ang3 accounting for 427 electrons was removed.
;
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         15693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1410
_reflns_number_gt                8464
_reflns_number_total             15693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b01445_si_001.cif
_cod_data_source_block           13114sq_complex2
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4129377