Cobalt azide complexes with a tris(carbene)borate ligand scaffold
Scepaniak, Jeremiah J.; Margarit, Charles G.; Bontchev, Ranko P.; Smith, Jeremy M.; Acta Crystallographica Section C 69 (2013) 968–971; doi:10.1107/S0108270113017022

data_2019156
_publ_section_title
;
 Cobalt azide complexes with a tris(carbene)borate ligand scaffold
;
_journal_coeditor_code           YP3036
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              968
_journal_page_last               971
_journal_paper_doi               10.1107/S0108270113017022
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Co (C27 H38 B N6) (N3)]'
_chemical_formula_moiety         'C27 H38 B Co N9'
_chemical_formula_sum            'C27 H38 B Co N9'
_chemical_formula_weight         558.40
_chemical_name_systematic
(Azido-\k<i>N</i>)[1,1,',1''-(phenylboranetriyl)tris(3-<i>tert</i>-butyl-1<i>H</i>-imidazol-2-ylidene)]cobalt(II)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.016(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8910(3)
_cell_length_b                   17.7415(5)
_cell_length_c                   16.1660(5)
_cell_measurement_temperature    223(2)
_cell_volume                     2835.07(15)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 20120)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0857
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50578
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(APEX2; Bruker, 2009)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.322
_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     361
_refine_ls_number_reflns         7050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.9210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                4482
_reflns_number_total             7050
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yp3036.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2019156
_cod_database_fobs_code          2019156