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_4033559
_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         'C64 H68 N2'
_chemical_formula_sum            'C64 H68 N2'
_chemical_formula_weight         865.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-03
_audit_creation_method
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.775(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3548(13)
_cell_length_b                   17.6188(8)
_cell_length_c                   19.186(2)
_cell_measurement_reflns_used    1256
_cell_measurement_temperature    292.84(10)
_cell_measurement_theta_max      20.6670
_cell_measurement_theta_min      3.5960
_cell_volume                     5019.6(8)
_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      air
_diffrn_ambient_temperature      292.84(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -14.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  -99.0000   90.0000 39

  2 omega   -8.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305    0.0000    0.0000 103

  3 omega  -23.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6305   19.0000  -90.0000 89
;
_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      0.0161508000
_diffrn_orient_matrix_UB_12      -0.0058676000
_diffrn_orient_matrix_UB_13      -0.0285918000
_diffrn_orient_matrix_UB_21      -0.0359849000
_diffrn_orient_matrix_UB_22      0.0221831000
_diffrn_orient_matrix_UB_23      -0.0261674000
_diffrn_orient_matrix_UB_31      0.0269641000
_diffrn_orient_matrix_UB_32      0.0330874000
_diffrn_orient_matrix_UB_33      0.0124007000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1191
_diffrn_reflns_av_unetI/netI     0.2063
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18505
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79366
_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    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         9858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.2261
_refine_ls_R_factor_gt           0.0850
_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^)+(0.0541P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.2327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3540
_reflns_number_total             9858
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00375_si_004.cif
_cod_data_source_block           xray_sx
_cod_depositor_comments          'Adding full bibliography for 4033559.cif.'
_cod_original_cell_volume        5019.5(8)
_cod_database_code               4033559
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.70
_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.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C80(H80A,H80B), C147(H14D,H14E), C162(H16A,H16B), C165(H16C,
 H16D), C184(H18A,H18B), C190(H19C,H19D), C201(H20A,H20B), C217(H21G,H21H),
 C219(H21I,H21J), C0AA(H0AA,H0AB), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C66(H66), C72(H72), C73(H73), C83(H83), C92(H92), C101(H101),
 C124(H124), C141(H141), C174(H174), C186(H186), C187(H187), C192(H192),
 C196(H196), C208(H208), C210(H210), C232(H232), C12(H12), C1AA(H1AA),
 C2AA(H2AA)
2.c Idealised Me refined as rotating group:
 C143(H14A,H14B,H14C), C211(H21A,H21B,H21C), C216(H21D,H21E,H21F), C225(H22A,
 H22B,H22C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C20(H20C,H20D,H20E),
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              97930
_shelx_hkl_checksum              13262
_olex2_date_sample_data_collection 2017-11-02
_olex2_submission_special_instructions 'No special instructions were received'