Photoactive Boron-Nitrogen-Carbon Hybrids: From Azo-borazines to Polymeric Materials.
Oubaha, Hamid; Demitri, Nicola; Rault-Berthelot, Joëlle; Dubois, Philippe; Coulembier, Olivier; Bonifazi, Davide; The Journal of organic chemistry 84 (2019) 9101–9116; doi:10.1021/acs.joc.9b01046

data_4034209
_publ_section_title
;
 Photoactive Boron-Nitrogen-Carbon Hybrids: From Azo-borazines to
 Polymeric Materials.
;
_journal_issue                   14
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9101
_journal_page_last               9116
_journal_paper_doi               10.1021/acs.joc.9b01046
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C78 H66 B3 N9'
_chemical_formula_sum            'C78 H66 B3 N9'
_chemical_formula_weight         1161.82
_chemical_name_common            Azo-borazine-3
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.56(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.221(4)
_cell_length_b                   20.797(4)
_cell_length_c                   15.506(3)
_cell_measurement_reflns_used    1497
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.452
_cell_measurement_theta_min      0.993
_cell_volume                     6514(2)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Ortep3 for Windows - Coot'
_computing_publication_material  'enCIFer - publCIF'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'Sir2014 (Burla, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            63056
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        24.624
_diffrn_reflns_theta_max         24.624
_diffrn_reflns_theta_min         0.993
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       'Thin plate'
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0108(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         11189
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.1017
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1813P)^2^+6.6961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2874
_refine_ls_wR_factor_ref         0.3449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6541
_reflns_number_total             11189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01046_si_004.cif
_cod_data_source_block           AzoBN3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4034209
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.993
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              34893
_shelx_hkl_checksum              2410