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_4035451
_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             2017-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.476(2)
_cell_length_b                   32.295(8)
_cell_length_c                   17.436(5)
_cell_measurement_reflns_used    5149
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.06
_cell_measurement_theta_min      2.34
_cell_volume                     5336(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.2136
_diffrn_reflns_Laue_measured_fraction_full 0.888
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22884
_diffrn_reflns_point_group_measured_fraction_full 0.769
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.227
_diffrn_reflns_theta_min         1.719
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_type   none
_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    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.012(7)
_refine_ls_extinction_coef       0.00043(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.531
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1266
_refine_ls_number_reflns         14861
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.531
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0374
_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^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    0.646
_reflns_Friedel_fraction_max     0.648
_reflns_number_gt                6293
_reflns_number_total             14861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00375_si_003.cif
_cod_data_source_block           sdd_170927_b_0m_pl
_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_database_code               4035451
_shelxl_version_number           2013-2
_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. Restrained distances
 H3A-N3
 0.8 with sigma of 0.01
 N3-H3B
 0.8 with sigma of 0.01
 H2B-N2
 0.8 with sigma of 0.01
 N2-H2A
 0.8 with sigma of 0.01
 H1A-N1
 0.8 with sigma of 0.01
 N1-H1B
 0.8 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C122) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C1G(H1GA,H1GB), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,
 H28B), C31(H31A,H31B), C88(H88A,H88B), C89(H89A,H89B), C91(H91A,H91B),
 C92(H92A,H92B), C94(H94A,H94B), C95(H95A,H95B), C56(H56A,H56B), C57(H57A,H57B),
  C59(H59A,H59B), C60(H60A,H60B), C62(H62A,H62B), C63(H63A,H63B), C120(H12A,
 H12B), C121(H12C,H12D), C123(H12H,H12I), C124(H12J,H12K), C126(H12O,H12P),
 C127(H12Q,H12R)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C21(H21), C68(H68), C71(H71), C75(H75), C76(H76), C77(H77), C78(H78),
  C82(H82), C83(H83), C84(H84), C85(H85), C36(H36), C37(H37), C38(H38),
 C39(H39), C43(H43), C46(H46), C50(H50), C51(H51), C52(H52), C53(H53),
 C100(H100), C103(H103), C107(H107), C108(H108), C109(H109), C110(H110),
 C114(H114), C115(H115), C116(H116), C117(H117)
4.c X=CH2 refined with riding coordinates:
 N4(H4A,H4B)
4.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C), C87(H87A,H87B,H87C), C90(H90A,H90B,H90C), C93(H93A,H93B,H93C), C96(H96A,
 H96B,H96C), C55(H55A,H55B,H55C), C58(H58A,H58B,H58C), C61(H61A,H61B,H61C),
 C64(H64A,H64B,H64C), C119(H11A,H11B,H11C), C122(H12E,H12F,H12G), C125(H12L,
 H12M,H12N), C128(H12S,H12T,H12U)
;
_shelx_res_checksum              9239
_shelx_hkl_checksum              1272
_olex2_submission_special_instructions 'No special instructions were received'