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_7041483
_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         'C25 H16 Br6'
_chemical_formula_sum            'C25 H16 Br6'
_chemical_formula_weight         795.84
_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             2014-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.806(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4708(4)
_cell_length_b                   9.3343(2)
_cell_length_c                   18.9329(5)
_cell_measurement_reflns_used    15779
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      25.8770
_cell_measurement_theta_min      1.8100
_cell_volume                     2377.78(11)
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_diffrn_measurement_details
;
  1 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000  -90.0000 98

  2 omega    3.00   95.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   38.0000 -150.0000 92

  3 omega    6.00   93.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   57.0000   30.0000 87

  4 omega    6.00   83.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926 -130.0000   22.5926 77

  5 omega  -46.00   47.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -38.0000   30.0000 93

  6 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000   90.0000 98

  7 omega  -46.00   47.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -38.0000  120.0000 93

  8 omega  -44.00   43.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -57.0000 -120.0000 87

  9 omega   35.00   99.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  178.0000   60.0000 64

 10 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000 -150.0000 98

 11 omega   -2.00   77.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926 -120.0000 -159.4549 79

 12 omega  -85.00   -8.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  135.0000   27.8271 77

 13 omega  -95.00   48.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -180.0000 143

 14 omega  -20.00   65.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -99.0000   60.0000 85

 15 omega  -20.00   65.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  -99.0000  -60.0000 85

 16 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000  120.0000 98

 17 omega    6.00   93.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   57.0000  -30.0000 87

 18 omega   -4.00   94.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   77.0000   30.0000 98

 19 omega    6.00   93.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926   57.0000   60.0000 87

 20 omega   35.00   99.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926  178.0000  -30.0000 64

 21 omega   34.00  100.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       24.7926 -178.0000  150.0000 66

 22 omega  -95.00   48.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -120.0000 143

 23 omega  -95.00   48.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -90.0000 143

 24 omega  -95.00   23.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -60.0000 118

 25 omega  -95.00   48.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -150.0000 143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0025697000
_diffrn_orient_matrix_UB_12      0.0636870000
_diffrn_orient_matrix_UB_13      0.0202831000
_diffrn_orient_matrix_UB_21      0.0467921000
_diffrn_orient_matrix_UB_22      0.0217228000
_diffrn_orient_matrix_UB_23      -0.0118876000
_diffrn_orient_matrix_UB_31      -0.0241285000
_diffrn_orient_matrix_UB_32      0.0353337000
_diffrn_orient_matrix_UB_33      -0.0292329000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            101948
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.814
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.144
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_type   gaussian
_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)
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    2.223
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.0815
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0217P)^2^+4.1154P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3834
_reflns_number_total             4684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04350j2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7041472--7041483.cif.'
_cod_original_cell_volume        2377.77(11)
_cod_database_code               7041483
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C25H16Br6 '
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C11(H11), C14(H14), C18(H18), C21(H21)
2.c Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c)
;
_olex2_exptl_crystal_mounting_method mounted