Poly-Lewis-acids based on bowl-shaped tribenzotriquinacene.
Tomaschautzky, Janek; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1112–1123; doi:10.1039/c6dt04350j

data_7041478
_publ_section_title
;
 Poly-Lewis-acids based on bowl-shaped tribenzotriquinacene.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1112
_journal_page_last               1123
_journal_paper_doi               10.1039/c6dt04350j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C46 H28'
_chemical_formula_sum            'C46 H28'
_chemical_formula_weight         580.68
_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             2015-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.901(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.7889(10)
_cell_length_b                   10.4654(4)
_cell_length_c                   27.3953(16)
_cell_measurement_reflns_used    5367
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.0450
_cell_measurement_theta_min      3.3450
_cell_volume                     6490.2(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9672
_diffrn_measurement_details
;
  1 omega  -49.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   90.0000 45

  2 omega -114.00  -14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000   90.0000 100

  3 omega   -7.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -90.0000 40

  4 omega   57.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000   60.0000 54

  5 omega   43.00   83.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -30.0000  -30.0000 40

  6 omega   41.00   82.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -45.0000  120.0000 41

  7 omega   65.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -45.0000   60.0000 29

  8 omega   87.00  173.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343   45.0000  -30.0000 86

  9 omega   38.00   74.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -30.0000  150.0000 36

 10 omega   63.00  133.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  -77.0000  -90.0000 70

 11 omega   94.00  176.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343  125.0000    0.0000 82

 12 omega   40.00  113.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      109.0343 -125.0000  120.0000 73
;
_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      -0.0436630000
_diffrn_orient_matrix_UB_12      -0.1127231000
_diffrn_orient_matrix_UB_13      -0.0143006000
_diffrn_orient_matrix_UB_21      -0.0450740000
_diffrn_orient_matrix_UB_22      0.0768781000
_diffrn_orient_matrix_UB_23      0.0182109000
_diffrn_orient_matrix_UB_31      -0.0263547000
_diffrn_orient_matrix_UB_32      0.0553874000
_diffrn_orient_matrix_UB_33      -0.0543382000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28358
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         75.46
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       plate
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.0211
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         11464
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0711
_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^)+(0.1235P)^2^+0.2845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.2171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7493
_reflns_number_total             11464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04350j2.cif
_cod_data_source_block           compound18
_cod_depositor_comments
'Adding full bibliography for 7041472--7041483.cif.'
_cod_database_code               7041478
_chemical_oxdiff_formula         'C48 H48'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_date_sample_data_collection 1428583816.21
_olex2_exptl_crystal_mounting_method mounted
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C84-C83 \\sim C76-C75 \\sim C92-C91 \\sim C38-C37 \\sim C46-C45 \\sim C30-C29
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C1(H1), C47(H47)
3.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), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C27(H27), C28(H28),
  C32(H32), C33(H33), C35(H35), C36(H36), C40(H40), C41(H41), C43(H43),
 C44(H44), C50(H50), C51(H51), C52(H52), C53(H53), C57(H57), C58(H58), C59(H59),
  C60(H60), C64(H64), C65(H65), C66(H66), C67(H67), C70(H70), C71(H71),
 C73(H73), C74(H74), C78(H78), C79(H79), C81(H81), C82(H82), C86(H86), C87(H87),
  C89(H89), C90(H90)
3.c :
 C30(H30), C38(H38), C46(H46), C76(H76), C84(H84), C92(H92)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2014/7