Bimetallic Cobalt-Dinitrogen Complexes: Impact of the Supporting Metal on N2 Activation.
Clouston, Laura J.; Bernales, Varinia; Carlson, Rebecca K.; Gagliardi, Laura; Lu, Connie C.; Inorganic chemistry 54 (2015) 9263–9270; doi:10.1021/acs.inorgchem.5b00983

data_4343503
_publ_section_title
;
 Bimetallic Cobalt-Dinitrogen Complexes: Impact of the Supporting Metal on
 N2 Activation.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9263
_journal_page_last               9270
_journal_paper_doi               10.1021/acs.inorgchem.5b00983
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         '2(C39 H60 N6 P3 Co Cr), 2(C18 H36 K N2 O6)'
_chemical_formula_sum            'C114 H192 Co2 Cr2 K2 N16 O12 P6'
_chemical_formula_weight         2464.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.0420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2453(3)
_cell_length_b                   31.9918(7)
_cell_length_c                   18.9780(4)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      74.43
_cell_measurement_theta_min      2.34
_cell_volume                     6801.1(3)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            106848
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.662
_diffrn_reflns_theta_min         2.337
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.831
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       needle
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Two molecules of pentane were removed from the asymmetric unit, consistent with the SQUEEZE results.
;
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.458(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1428
_refine_ls_number_reflns         27151
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0692P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.963
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                23744
_reflns_number_total             27151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00983_si_001.cif
_cod_data_source_block           13111sqz_compound_3
_cod_depositor_comments
'Adding full bibliography for 4343501--4343503.cif.'
_cod_original_formula_sum        'C114 H192 Co2 Cr2 K2 N16 O12 P6 '
_cod_database_code               4343503
_shelxl_version_number           2013-2
_shelx_res_checksum              3327
_shelx_hkl_checksum              25307