Quasi-planar diazadithio and diazodiseleno[8]circulenes: synthesis, structures and properties
Xiong, Xiaodong; Deng, Chun-Lin; Li, Zhiming; Peng, Xiao-Shui; Wong, Henry N. C.; Organic Chemistry Frontiers 4 (2017) 682–; doi:10.1039/C6QO00662K

data_1553594
_publ_section_title
;
 Quasi-planar diazadithio and diazodiseleno[8]circulenes: synthesis,
 structures and properties
;
_journal_issue                   5
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              682
_journal_paper_doi               10.1039/C6QO00662K
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C32 H22 Br8 N2'
_chemical_formula_weight         1073.79
_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-2014/6
_audit_update_record
;
2016-10-26 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                100.306(2)
_cell_angle_beta                 91.280(2)
_cell_angle_gamma                108.652(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8503(5)
_cell_length_b                   12.4427(5)
_cell_length_c                   12.9897(5)
_cell_measurement_reflns_used    410
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     1628.82(12)
_computing_cell_refinement       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_collection       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_reduction        'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEAG SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35914
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.762
_exptl_absorpt_coefficient_mu    9.875
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4105
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.189
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.433
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5893
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+5.3065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4687
_reflns_number_total             5893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qo00662k2.cif
_cod_data_source_block           xxd2191
_cod_database_code               1553594
_shelx_estimated_absorpt_t_min   0.110
_shelx_estimated_absorpt_t_max   0.243
_shelxl_version_number           2014/6
_shelx_res_checksum              17267
_shelx_hkl_checksum              56017