Intramolecular Hydride Transfer Reactions in (Formazanate)Boron Dihydride Complexes
Chang, Mu-Chieh; Otten, Edwin; Organometallics 35 (2016) 534–; doi:10.1021/acs.organomet.5b00968

data_4088260
_publ_section_title
;
 Intramolecular Hydride Transfer Reactions in (Formazanate)Boron Dihydride
 Complexes
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              534
_journal_paper_doi               10.1021/acs.organomet.5b00968
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C20 H19 B N4'
_chemical_formula_weight         326.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 94.7599(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.14730(10)
_cell_length_b                   20.9249(7)
_cell_length_c                   19.0650(6)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      3.895
_cell_volume                     1648.79(9)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16573
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         3.761
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  ?\0.7455
_exptl_absorpt_correction_T_min  0.6987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 1371 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.0(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.6185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.855
_reflns_Friedel_fraction_max     0.832
_reflns_number_gt                3193
_reflns_number_total             3350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00968_si_001.cif
_cod_data_source_block           mo_molan309_0m
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4088260
_shelx_estimated_absorpt_t_min   0.9350
_shelx_estimated_absorpt_t_max   0.9980
_shelxl_version_number           2014/6
_shelx_res_checksum              74513
_shelx_hkl_checksum              41416