Biconcave and Convex-Concave Tribenzotriquinacene Dimers.
Li, Zhi-Min; Li, Ya-Wei; Cao, Xiao-Ping; Chow, Hak-Fun; Kuck, Dietmar; The Journal of organic chemistry 83 (2018) 3433–3440; doi:10.1021/acs.joc.8b00375

data_4035452
_publ_section_title
;
 Biconcave and Convex-Concave Tribenzotriquinacene Dimers.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3433
_journal_page_last               3440
_journal_paper_doi               10.1021/acs.joc.8b00375
_journal_volume                  83
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H36 Br N'
_chemical_formula_sum            'C32 H36 Br N'
_chemical_formula_weight         514.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.412(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4747(3)
_cell_length_b                   32.2996(16)
_cell_length_c                   17.4267(9)
_cell_measurement_reflns_used    2066
_cell_measurement_temperature    293.70(10)
_cell_measurement_theta_max      19.7000
_cell_measurement_theta_min      3.6770
_cell_volume                     5332.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.70(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
  1 omega   30.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  -99.0000  -90.0000 34

  2 omega  -49.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  -19.0000 -120.0000 120

  3 omega  -11.00   15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -99.0000 -180.0000 26

  4 omega  -19.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -77.0000 -180.0000 74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0052298000
_diffrn_orient_matrix_UB_12      -0.0218569000
_diffrn_orient_matrix_UB_13      -0.0026855000
_diffrn_orient_matrix_UB_21      0.0351029000
_diffrn_orient_matrix_UB_22      -0.0005637000
_diffrn_orient_matrix_UB_23      0.0360818000
_diffrn_orient_matrix_UB_31      -0.0659112000
_diffrn_orient_matrix_UB_32      -0.0020470000
_diffrn_orient_matrix_UB_33      0.0186520000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.1740
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23233
_diffrn_reflns_point_group_measured_fraction_full 0.826
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.315
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1944 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1245
_refine_ls_number_reflns         17145
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1862
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0078P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.655
_reflns_Friedel_fraction_full    0.673
_reflns_Friedel_fraction_max     0.657
_reflns_number_gt                7897
_reflns_number_total             17145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00375_si_002.cif
_cod_data_source_block           lizhm_1010_dcm
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'AD' was changed
to 'ad' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5333.0(4)
_cod_database_code               4035452
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Br'
_reflns_odcompleteness_completeness 96.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 N1(H1A,H1B), N3(H3A,H3B), N2(H2A,H2B), N4(H4A,H4B)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C19(H19A,H19B), C20(H20A,H20B), C26(H26A,
 H26B), C27(H27A,H27B), C68(H68A,H68B), C69(H69A,H69B), C74(H74A,H74B),
 C75(H75A,H75B), C79(H79A,H79B), C80(H80A,H80B), C42(H42A,H42B), C43(H43A,H43B),
  C49(H49A,H49B), C50(H50A,H50B), C56(H56A,H56B), C57(H57A,H57B), C120(H12C,
 H12D), C121(H12E,H12F), C126(H12M,H12N), C127(H12O,H12P), C129(H12T,H12U),
 C130(H13C,H13D)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
 C25(H25), C29(H29), C32(H32), C85(H85), C88(H88), C89(H89), C90(H90), C91(H91),
  C92(H92), C93(H93), C94(H94), C95(H95), C96(H96), C45(H45), C48(H48),
 C52(H52), C53(H53), C54(H54), C55(H55), C59(H59), C60(H60), C61(H61), C62(H62),
  C108(H108), C109(H109), C110(H110), C111(H111), C112(H112), C113(H113),
 C114(H114), C115(H115), C116(H116), C119(H119)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C70(H70A,H70B,H70C), C76(H76A,H76B,H76C), C81(H81A,H81B,H81C), C84(H84A,
 H84B,H84C), C44(H44A,H44B,H44C), C51(H51A,H51B,H51C), C58(H58A,H58B,H58C),
 C64(H64A,H64B,H64C), C122(H12G,H12H,H12I), C123(H12J,H12K,H12L), C128(H12Q,
 H12R,H12S), C3AA(H3AA,H3AB,H3AC)
;
_shelx_res_checksum              85510
_shelx_hkl_checksum              4293
_olex2_date_sample_data_collection 2017-10-13
_olex2_submission_special_instructions 'No special instructions were received'