Arylallenes and the Halogeno-B(C6F5)2 Reagents: Facile Formation of 2-Borylindenes
Tao, Xin; Daniliuc, Constantin Gabriel; Soloviova, Kateryna; Strassert, Cristian Alejandro; Kehr, Gerald; Erker, Gerhard; Chemical Communications  (2019) –; doi:10.1039/C9CC04199K

data_7123940
_publ_section_title
;
 Arylallenes and the Halogeno-B(C6F5)2 Reagents: Facile Formation of
 2-Borylindenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04199K
_journal_year                    2019
_chemical_formula_sum            'C66 H24 B3 F30 N3'
_chemical_formula_weight         1461.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'APEX3 v2016.1-0'
_audit_update_record
;
2019-04-03 deposited with the CCDC.    2019-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.1620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2599(7)
_cell_length_b                   26.5169(9)
_cell_length_c                   13.8464(4)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.70
_cell_volume                     6677.2(4)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection
;

Collect (Nonius B.V., 1998)
;
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'rotating anode Nonius FR591'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.1043
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27433
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.75
_diffrn_source                   'Mo rotating anode'
_diffrn_source_type              'Mo rotating anode'
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.325
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1302
_refine_ls_number_reflns         11481
_refine_ls_number_restraints     1264
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.1224
_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^)+(0.0349P)^2^+36.7323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2223
_refine_ls_wR_factor_ref         0.2599
_reflns_number_gt                6701
_reflns_number_total             11481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04199k2.cif
_cod_data_source_block           erk9457
_cod_database_code               7123940
_shelx_res_checksum              61031
_shelx_fab_checksum              97043