Synthesis, structure and properties of C3-symmetric heterosuperbenzene with three BN units
Xiao-Ye Wang; Fang-Dong Zhuang; Xin-Chang Wang; Xiao-Yu Cao; Jie-Yu Wang; Jian Pei; Chem.Commun. 51 (2015) 4368–; doi:10.1039/C4cc10105G

data_7116643
_publ_section_title
;
 Synthesis, structure and properties of C3-symmetric heterosuperbenzene
 with three BN units
;
_journal_name_full               Chem.Commun.
_journal_page_first              4368
_journal_paper_doi               10.1039/C4cc10105G
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C42 H36 B3 N3 O6'
_chemical_formula_sum            'C42 H36 B3 N3 O6'
_chemical_formula_weight         711.17
_chemical_name_systematic        BN-Coronene
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-12-15 deposited with the CCDC.
2015-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                83.135(2)
_cell_angle_beta                 87.475(2)
_cell_angle_gamma                89.797(2)
_cell_formula_units_Z            4
_cell_length_a                   7.3418(2)
_cell_length_b                   15.7880(5)
_cell_length_c                   31.0079(8)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.6640
_cell_measurement_theta_min      4.2170
_cell_volume                     3564.96(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3415
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1357380000
_diffrn_orient_matrix_UB_12      -0.0023764000
_diffrn_orient_matrix_UB_13      -0.0391647000
_diffrn_orient_matrix_UB_21      0.0037521000
_diffrn_orient_matrix_UB_22      0.0982543000
_diffrn_orient_matrix_UB_23      -0.0069150000
_diffrn_orient_matrix_UB_31      0.1602410000
_diffrn_orient_matrix_UB_32      -0.0000634000
_diffrn_orient_matrix_UB_33      0.0304520000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            25470
_diffrn_reflns_point_group_measured_fraction_full 0.587
_diffrn_reflns_point_group_measured_fraction_max 0.562
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.932
_diffrn_reflns_theta_min         3.314
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1969
_refine_ls_number_reflns         16692
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0776P)^2^+3.5670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1871
_reflns_Friedel_coverage         0.165
_reflns_Friedel_fraction_full    0.175
_reflns_Friedel_fraction_max     0.159
_reflns_number_gt                14607
_reflns_number_total             16692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc10105g2.cif
_cod_data_source_block           exp_5449
_cod_original_cell_volume        3564.96(17)
_cod_database_code               7116643
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.46
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N20(H20), N23(H23), N26(H26), N28(H28), N29(H29), N30(H30), N31(H31),
 N33(H33), N1(H1), N3(H3), N6(H6), N9(H9), C14(H14), C31(H31A), C33(H33A),
 C34(H34), C41(H41), C47(H47), C50(H50), C53(H53), C56(H56), C3(H3A), C1B(H1B),
 C1C(H1C), C1D(H1D), C1F(H1F), C1G(H1G), C1J(H1J), C1K(H1K), C1L(H1L), C1V(H1V),
  C2A(H2A), C2G(H2G), C2K(H2K), C2M(H2M), C2W(H2W), C60(H60), C62(H62),
 C67(H67), C68(H68), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C85(H85), C86(H86),
 C87(H87), C89(H89), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96),
  C97(H97), C99(H99), C100(H100), C101(H101), C103(H103), C105(H105),
 C106(H106), C108(H108), C109(H109), C111(H111), C112(H112)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C35(H35A,H35B,H35C), C45(H45A,H45B,H45C), C51(H51A,H51B,
 H51C), C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C6(H6A,H6B,H6C), C1R(H1RA,
 H1RB,H1RC), C1Y(H1YA,H1YB,H1YC), C1Z(H1ZA,H1ZB,H1ZC), C2B(H2BA,H2BB,H2BC),
 C2D(H2DA,H2DB,H2DC), C65(H65A,H65B,H65C), C76(H76A,H76B,H76C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C98(H98A,
 H98B,H98C), C102(H10A,H10B,H10C), C104(H10D,H10E,H10F), C107(H10G,H10H,H10I),
 C110(H11A,H11B,H11C), C113(H11D,H11E,H11F)
;
_shelx_res_checksum              95837