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_4035450
_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_formula_moiety         '4(C H Cl3), 2(C32 H34 N)'
_chemical_formula_sum            'C68 H72 Cl12 N2'
_chemical_formula_weight         1342.67
_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
_audit_creation_date             2017-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.866(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.242(2)
_cell_length_b                   11.0682(6)
_cell_length_c                   20.7564(12)
_cell_measurement_reflns_used    3406
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      21.5020
_cell_measurement_theta_min      3.7170
_cell_volume                     6791.8(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   48.00   80.25   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  178.0000    0.0000 43

  2 omega   73.00   99.25   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  178.0000 -180.0000 35

  3 omega   42.00   68.25   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  178.0000  -30.0000 35

  4 omega    0.00   59.25   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305   57.0000 -150.0000 79

  5 omega  -45.00   79.50   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305  -19.0000    0.0000 166
;
_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      -0.0194504000
_diffrn_orient_matrix_UB_12      0.0308635000
_diffrn_orient_matrix_UB_13      -0.0208289000
_diffrn_orient_matrix_UB_21      -0.0135478000
_diffrn_orient_matrix_UB_22      -0.0508520000
_diffrn_orient_matrix_UB_23      0.0012550000
_diffrn_orient_matrix_UB_31      -0.0036474000
_diffrn_orient_matrix_UB_32      0.0239257000
_diffrn_orient_matrix_UB_33      0.0294823000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.1345
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29733
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.382
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         13315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.2170
_refine_ls_R_factor_gt           0.1318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3449
_refine_ls_wR_factor_ref         0.4114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6165
_reflns_number_total             13315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00375_si_005.cif
_cod_data_source_block           lizhm_1110
_cod_original_cell_volume        6791.8(8)
_cod_database_code               4035450
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.68
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C62(0.75) C63(0.75) C62'(0.25) C63'(0.25)
3.a Ternary CH refined with riding coordinates:
 C64(H64), C65(H65), C66(H66), C67(H67)
3.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,
 H30B), C31(H31A,H31B), C54(H54A,H54B), C55(H55A,H55B), C58(H58A,H58B),
 C59(H59A,H59B), C61(H61A,H61B), C62(H62A,H62B)
3.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C50(H50), C53(H53)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C60(H60A,H60B,H60C), C63(H63A,
 H63B,H63C)
;
_shelx_res_checksum              96310
_shelx_hkl_checksum              14830
_olex2_date_sample_data_collection 2017-11-10
_olex2_submission_special_instructions 'No special instructions were received'