Complexation and Release of N-Heterocyclic Carbene-Aminoborylene Ligands from Group VI and VIII Metals.
Pranckevicius, Conor; Jimenéz-Halla, J Oscar C; Kirsch, Marius; Krummenacher, Ivo; Braunschweig, Holger; Journal of the American Chemical Society 140 (2018) 10524–10529; doi:10.1021/jacs.8b05398

data_4132661
_publ_section_title
;
 Complexation and Release of N-Heterocyclic Carbene-Aminoborylene Ligands
 from Group VI and VIII Metals.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10524
_journal_page_last               10529
_journal_paper_doi               10.1021/jacs.8b05398
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C63 H76 B Cu F3 Fe N5 O7 S'
_chemical_formula_sum            'C63 H76 B Cu F3 Fe N5 O7 S'
_chemical_formula_weight         1234.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2348(13)
_cell_length_b                   11.0028(7)
_cell_length_c                   29.4015(15)
_cell_measurement_reflns_used    2926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.05
_cell_measurement_theta_min      2.24
_cell_volume                     6222.4(7)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'Mercury 2017'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_number            6441
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_min         2.531
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_correction_T_min  0.383518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   twin-abs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         6441
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0597P)^2^+4.4099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                5598
_reflns_number_total             6441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05398_si_002.cif
_cod_data_source_block           copr006_0ma
_cod_depositor_comments
;

2020-10-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum
'C21 H25.33 B0.33 Cu0.33 F Fe0.33 N1.67 O2.33 S0.33'
_cod_original_formula_weight         411.51
_cod_original_formula_moiety
'C21 H25.33 B0.33 Cu0.33 F Fe0.33 N1.67 O2.33 S0.33'
_cod_original_formula_units_Z            12
_cod_database_code               4132661
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              97768
_shelx_hkl_checksum              49375