Zirconocene-Based Methods for the Preparation of BN-Indenes: Application to the Synthesis of 1,5-Dibora-4a,8a-diaza-1,2,3,5,6,7-hexaaryl-4,8-dimethyl-s-indacenes
Morgan, Matthew M.; Patrick, Evan A.; Rautiainen, J. Mikko; Tuononen, Heikki M.; Piers, Warren E.; Spasyuk, Denis M.; Organometallics  (2017) –; doi:10.1021/acs.organomet.7b00051

data_4087172
_publ_section_title
;
 Zirconocene-Based Methods for the Preparation of BN-Indenes: Application
 to the Synthesis of
 1,5-Dibora-4a,8a-diaza-1,2,3,5,6,7-hexaaryl-4,8-dimethyl-s-indacenes
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.7b00051
_journal_year                    2017
_chemical_formula_moiety         ' C46 H36 B2 Cl2 N2 '
_chemical_formula_sum            'C46 H36 B2 Cl2 N2'
_chemical_formula_weight         709.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                112.9650(10)
_cell_angle_beta                 113.3580(10)
_cell_angle_gamma                100.9890(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4818(3)
_cell_length_b                   14.8376(3)
_cell_length_c                   15.0664(5)
_cell_measurement_reflns_used    5826
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.54
_cell_measurement_theta_min      3.54
_cell_volume                     2497.76(12)
_computing_publication_material  'LinXTL v.  5.3.1'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26411
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.829
_diffrn_reflns_theta_min         3.544
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         9422
_refine_ls_number_restraints     450
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0681P)^2^+0.1358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8400
_reflns_number_total             9422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00051_si_002.cif
_cod_data_source_block           mm1522_a
_cod_depositor_comments
;

2020-10-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2497.76(11)
_cod_original_formula_sum        'C23 H18 B Cl N'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     354.64
_cod_database_code               4087172
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.772
_shelxl_version_number           2014/6
_shelx_res_checksum              41284
_shelx_hkl_checksum              44573