Isolable Borane-Based Diradical and Triradical Fused by a Diamagnetic Transition Metal Ion.
Wang, Lei; Li, Jing; Zhang, Li; Fang, Yong; Chen, Chao; Zhao, Yue; Song, You; Deng, Liang; Tan, Gengwen; Wang, Xinping; Power, Philip P.; Journal of the American Chemical Society 139 (2017) 17723–17726; doi:10.1021/jacs.7b10141

data_4131753
_publ_section_title
;
 Isolable Borane-Based Diradical and Triradical Fused by a Diamagnetic
 Transition Metal Ion.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17723
_journal_page_last               17726
_journal_paper_doi               10.1021/jacs.7b10141
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C138 H150 B6 Fe N6, C20 H40 K O8, 4(C4 H8 O)'
_chemical_formula_sum            'C174 H222 B6 Fe K N6 O12'
_chemical_formula_weight         2749.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.974(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.6500(18)
_cell_length_b                   17.6690(12)
_cell_length_c                   31.499(2)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.43
_cell_volume                     15864.7(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep 3v2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            54151
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.305
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5916
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.689
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         13930
_refine_ls_number_restraints     3379
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+48.5800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12031
_reflns_number_total             13930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10141_si_003.cif
_cod_data_source_block           2_a
_cod_original_cell_volume        15864.9(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4131753
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              16488
_shelx_hkl_checksum              57734