Cobalt(II) Complex of a Diazoalkane Radical Anion.
Bonyhady, Simon J.; Goldberg, Jonathan M.; Wedgwood, Nicole; Dugan, Thomas R.; Eklund, Andrew G.; Brennessel, William W.; Holland, Patrick L.; Inorganic chemistry 54 (2015) 5148–5150; doi:10.1021/acs.inorgchem.5b00673

data_4346161
_publ_section_title
;
 Cobalt(II) Complex of a Diazoalkane Radical Anion.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5148
_journal_page_last               5150
_journal_paper_doi               10.1021/acs.inorgchem.5b00673
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H63 Co N3'
_chemical_formula_sum            'C48 H63 Co N3'
_chemical_formula_weight         740.94
_chemical_name_common            holtd37
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 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                 97.137(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.623(2)
_cell_length_b                   9.6011(18)
_cell_length_c                   17.401(3)
_cell_measurement_reflns_used    4011
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      26.95
_cell_measurement_theta_min      2.43
_cell_volume                     2092.6(6)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.1014
_diffrn_reflns_av_sigmaI/netI    0.1447
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51481
_diffrn_reflns_theta_full        33.73
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.9652
_exptl_absorpt_correction_T_min  0.8930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'dark orange-brown'
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
'Flack H D (1983), 7912 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.032(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         16673
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1522
_reflns_number_gt                10312
_reflns_number_total             16673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00673_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        2092.5(7)
_cod_database_code               4346161