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_4131754
_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'
_chemical_formula_sum            'C138 H150 B6 Fe N6'
_chemical_formula_weight         2013.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                82.992(2)
_cell_angle_beta                 82.381(3)
_cell_angle_gamma                73.241(3)
_cell_formula_units_Z            2
_cell_length_a                   14.0035(12)
_cell_length_b                   17.0728(14)
_cell_length_c                   28.873(2)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.38
_cell_volume                     6525.8(9)
_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    'SHELXS-2014/7 (Sheldrick 2014)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.1254
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            47414
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.980
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1477
_refine_ls_number_reflns         22914
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0771
_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^)+(0.0960P)^2^+4.7580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1897
_refine_ls_wR_factor_ref         0.2228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12938
_reflns_number_total             22914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10141_si_002.cif
_cod_data_source_block           1_a_sq
_cod_original_cell_volume        6525.9(10)
_cod_database_code               4131754
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              28207
_shelx_hkl_checksum              6776
_shelx_fab_checksum              31435