#------------------------------------------------------------------------------
#$Date: 2017-01-07 04:23:26 +0200 (Sat, 07 Jan 2017) $
#$Revision: 189992 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/19/2241996.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241996
loop_
_publ_author_name
'Kamata, Sho'
'Sato, Sota'
'Wu, Jishan'
'Isobe, Hiroyuki'
_publ_section_title
;
 Crystal structure of
 7,15-bis(4-tert-butylphenyl)-1,9-dimethylheptazethrene
;
_journal_coeditor_code           IS5468
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              99
_journal_page_last               102
_journal_paper_doi               10.1107/S2056989016020247
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C50 H44'
_chemical_formula_moiety         'C50 H44'
_chemical_formula_sum            'C50 H44'
_chemical_formula_weight         644.90
_chemical_name_systematic
;
7,15-Bis(4-tert-butylphenyl)-1,9-dimethylheptazethrene
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.874(2)
_cell_angle_beta                 95.080(2)
_cell_angle_gamma                115.249(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7644(2)
_cell_length_b                   9.2002(3)
_cell_length_c                   13.1212(3)
_cell_measurement_reflns_used    15939
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      3.58
_cell_volume                     894.47(5)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2016) and Mercury (Macrae et al.,
2008)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2016),
OLEX2 (Dolomanov et al.,  2009) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016  (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22866
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         3.604
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             344.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0807P)²+0.1872P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                2930
_reflns_number_total             3256
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            is5468sup1.cif
_cod_data_source_block           I
_cod_database_code               2241996
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
C C1 0.77143(15) 0.27792(16) 0.37967(10) 0.0282(3) Uani d 1
C C2 0.82438(16) 0.19027(16) 0.29671(11) 0.0304(3) Uani d 1
H H2 0.901044 0.149216 0.316696 0.036 Uiso calc 1
C C3 0.77086(16) 0.16138(16) 0.18882(11) 0.0294(3) Uani d 1
H H3 0.802444 0.093561 0.135216 0.035 Uiso calc 1
C C3A 0.66842(15) 0.23267(15) 0.15725(10) 0.0270(3) Uani d 1
C C3A1 0.61706(14) 0.32728(14) 0.23942(10) 0.0247(3) Uani d 1
C C4 0.61937(16) 0.21352(16) 0.04656(10) 0.0299(3) Uani d 1
H H4 0.651358 0.147501 -0.007973 0.036 Uiso calc 1
C C5 0.52627(16) 0.28945(16) 0.01768(10) 0.0308(3) Uani d 1
H H5 0.492798 0.274895 -0.056770 0.037 Uiso calc 1
C C6 0.48038(16) 0.38832(16) 0.09751(10) 0.0284(3) Uani d 1
H H6 0.418515 0.442753 0.076400 0.034 Uiso calc 1
C C6A 0.52289(15) 0.40922(15) 0.20719(10) 0.0254(3) Uani d 1
C C7 0.47383(15) 0.51085(15) 0.28851(10) 0.0253(3) Uani d 1
C C7A 0.49880(15) 0.51364(15) 0.39461(10) 0.0255(3) Uani d 1
C C8 0.42937(15) 0.59605(15) 0.47208(10) 0.0261(3) Uani d 1
H H8 0.386896 0.666232 0.452300 0.031 Uiso calc 1
C C8A 0.57990(15) 0.41936(15) 0.42770(10) 0.0249(3) Uani d 1
C C8B 0.65887(15) 0.34037(15) 0.35078(10) 0.0255(3) Uani d 1
C C1M 0.84692(17) 0.29973(19) 0.49464(11) 0.0359(3) Uani d 1
H H1M1 0.953456 0.288760 0.496403 0.054 Uiso calc 1
H H1M2 0.762462 0.211359 0.517639 0.054 Uiso calc 1
H H1M3 0.873653 0.413186 0.544212 0.054 Uiso calc 1
C C1P 0.37768(15) 0.59823(15) 0.25632(9) 0.0257(3) Uani d 1
C C2P 0.45677(15) 0.77354(16) 0.27639(10) 0.0275(3) Uani d 1
H H2P 0.578450 0.840095 0.305958 0.033 Uiso calc 1
C C3P 0.36053(16) 0.85288(16) 0.25386(10) 0.0278(3) Uani d 1
H H3P 0.418003 0.972795 0.268045 0.033 Uiso calc 1
C C4P 0.18176(15) 0.76070(15) 0.21096(10) 0.0273(3) Uani d 1
C C5P 0.10460(16) 0.58447(16) 0.18943(11) 0.0329(3) Uani d 1
H H5P -0.016815 0.517320 0.158986 0.039 Uiso calc 1
C C6P 0.19987(16) 0.50500(16) 0.21115(11) 0.0317(3) Uani d 1
H H6P 0.142991 0.384575 0.194958 0.038 Uiso calc 1
C C1T 0.06794(16) 0.84316(17) 0.19069(11) 0.0333(3) Uani d 1
C C2T -0.05461(19) 0.8203(2) 0.26853(15) 0.0468(4) Uani d 1
H H2T1 -0.118334 0.698859 0.259859 0.070 Uiso calc 1
H H2T2 -0.137001 0.861074 0.251474 0.070 Uiso calc 1
H H2T3 0.013342 0.886463 0.343903 0.070 Uiso calc 1
C C3T 0.17399(17) 1.03289(17) 0.20891(13) 0.0401(3) Uani d 1
H H3T1 0.096047 1.078314 0.191671 0.060 Uiso calc 1
H H3T2 0.255721 1.048167 0.161518 0.060 Uiso calc 1
H H3T3 0.238494 1.094359 0.285279 0.060 Uiso calc 1
C C4T -0.04149(19) 0.7524(2) 0.07259(13) 0.0465(4) Uani d 1
H H4T1 -0.118581 0.631892 0.061158 0.070 Uiso calc 1
H H4T2 0.035486 0.759603 0.022257 0.070 Uiso calc 1
H H4T3 -0.111104 0.807899 0.059085 0.070 Uiso calc 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle
C2 C1 C8B . 118.76(11)
C2 C1 C1M . 115.40(11)
C8B C1 C1M . 125.82(11)
C3 C2 C1 . 123.15(12)
C3 C2 H2 . 118.4
C1 C2 H2 . 118.4
C2 C3 C3A . 119.76(12)
C2 C3 H3 . 120.1
C3A C3 H3 . 120.1
C3 C3A C4 . 121.12(11)
C3 C3A C3A1 . 118.58(11)
C4 C3A C3A1 . 120.30(11)
C3A C3A1 C8B . 120.68(11)
C3A C3A1 C6A . 118.01(11)
C8B C3A1 C6A . 121.30(11)
C5 C4 C3A . 120.49(11)
C5 C4 H4 . 119.8
C3A C4 H4 . 119.8
C4 C5 C6 . 120.12(11)
C4 C5 H5 . 119.9
C6 C5 H5 . 119.9
C6A C6 C5 . 121.78(12)
C6A C6 H6 . 119.1
C5 C6 H6 . 119.1
C6 C6A C3A1 . 119.22(11)
C6 C6A C7 . 121.14(11)
C3A1 C6A C7 . 119.64(11)
C7A C7 C6A . 120.21(11)
C7A C7 C1P . 119.24(11)
C6A C7 C1P . 120.20(10)
C7 C7A C8 . 120.18(11)
C7 C7A C8A . 121.18(11)
C8 C7A C8A . 118.35(11)
C8A C8 C7A 2_666 124.58(11)
C8A C8 H8 2_666 117.7
C7A C8 H8 . 117.7
C8 C8A C7A 2_666 116.82(11)
C8 C8A C8B 2_666 124.06(11)
C7A C8A C8B . 119.05(11)
C1 C8B C3A1 . 118.48(11)
C1 C8B C8A . 124.42(11)
C3A1 C8B C8A . 117.10(11)
C1 C1M H1M1 . 109.5
C1 C1M H1M2 . 109.5
H1M1 C1M H1M2 . 109.5
C1 C1M H1M3 . 109.5
H1M1 C1M H1M3 . 109.5
H1M2 C1M H1M3 . 109.5
C2P C1P C6P . 117.68(11)
C2P C1P C7 . 122.52(11)
C6P C1P C7 . 119.66(11)
C3P C2P C1P . 121.00(11)
C3P C2P H2P . 119.5
C1P C2P H2P . 119.5
C2P C3P C4P . 121.54(11)
C2P C3P H3P . 119.2
C4P C3P H3P . 119.2
C3P C4P C5P . 116.84(11)
C3P C4P C1T . 123.67(11)
C5P C4P C1T . 119.45(11)
C6P C5P C4P . 121.80(11)
C6P C5P H5P . 119.1
C4P C5P H5P . 119.1
C5P C6P C1P . 121.12(12)
C5P C6P H6P . 119.4
C1P C6P H6P . 119.4
C3T C1T C4P . 112.58(10)
C3T C1T C2T . 109.31(12)
C4P C1T C2T . 108.22(11)
C3T C1T C4T . 108.22(11)
C4P C1T C4T . 109.63(11)
C2T C1T C4T . 108.82(12)
C1T C2T H2T1 . 109.5
C1T C2T H2T2 . 109.5
H2T1 C2T H2T2 . 109.5
C1T C2T H2T3 . 109.5
H2T1 C2T H2T3 . 109.5
H2T2 C2T H2T3 . 109.5
C1T C3T H3T1 . 109.5
C1T C3T H3T2 . 109.5
H3T1 C3T H3T2 . 109.5
C1T C3T H3T3 . 109.5
H3T1 C3T H3T3 . 109.5
H3T2 C3T H3T3 . 109.5
C1T C4T H4T1 . 109.5
C1T C4T H4T2 . 109.5
H4T1 C4T H4T2 . 109.5
C1T C4T H4T3 . 109.5
H4T1 C4T H4T3 . 109.5
H4T2 C4T H4T3 . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 C2 . 1.4068(18)
C1 C8B . 1.4084(17)
C1 C1M . 1.5159(17)
C2 C3 . 1.3655(18)
C2 H2 . 0.9500
C3 C3A . 1.4117(17)
C3 H3 . 0.9500
C3A C4 . 1.4178(17)
C3A C3A1 . 1.4247(17)
C3A1 C8B . 1.4335(17)
C3A1 C6A . 1.4394(17)
C4 C5 . 1.3689(18)
C4 H4 . 0.9500
C5 C6 . 1.3970(18)
C5 H5 . 0.9500
C6 C6A . 1.3926(17)
C6 H6 . 0.9500
C6A C7 . 1.4409(17)
C7 C7A . 1.3813(17)
C7 C1P . 1.4952(16)
C7A C8 . 1.4353(17)
C7A C8A . 1.4572(16)
C8 C8A 2_666 1.3664(17)
C8 H8 . 0.9500
C8A C8B . 1.4756(17)
C1M H1M1 . 0.9800
C1M H1M2 . 0.9800
C1M H1M3 . 0.9800
C1P C2P . 1.3902(17)
C1P C6P . 1.3905(17)
C2P C3P . 1.3896(17)
C2P H2P . 0.9500
C3P C4P . 1.3928(17)
C3P H3P . 0.9500
C4P C5P . 1.3950(17)
C4P C1T . 1.5331(17)
C5P C6P . 1.3804(17)
C5P H5P . 0.9500
C6P H6P . 0.9500
C1T C3T . 1.5220(18)
C1T C2T . 1.5361(19)
C1T C4T . 1.538(2)
C2T H2T1 . 0.9800
C2T H2T2 . 0.9800
C2T H2T3 . 0.9800
C3T H3T1 . 0.9800
C3T H3T2 . 0.9800
C3T H3T3 . 0.9800
C4T H4T1 . 0.9800
C4T H4T2 . 0.9800
C4T H4T3 . 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C3P H3P Cg1 1_565 0.95 2.80 3.6278(15) 147
C3T H3T2 Cg2 1_565 0.98 2.97 3.7929(17) 143
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C8B C1 C2 C3 . . -0.49(19)
C1M C1 C2 C3 . . -179.09(12)
C1 C2 C3 C3A . . 5.13(19)
C2 C3 C3A C4 . . 176.25(11)
C2 C3 C3A C3A1 . . -2.76(17)
C3 C3A C3A1 C8B . . -4.01(17)
C4 C3A C3A1 C8B . . 176.97(10)
C3 C3A C3A1 C6A . . 175.79(10)
C4 C3A C3A1 C6A . . -3.22(17)
C3 C3A C4 C5 . . -177.21(11)
C3A1 C3A C4 C5 . . 1.78(18)
C3A C4 C5 C6 . . 0.71(18)
C4 C5 C6 C6A . . -1.71(19)
C5 C6 C6A C3A1 . . 0.18(18)
C5 C6 C6A C7 . . -179.66(11)
C3A C3A1 C6A C6 . . 2.25(16)
C8B C3A1 C6A C6 . . -177.94(10)
C3A C3A1 C6A C7 . . -177.91(10)
C8B C3A1 C6A C7 . . 1.89(17)
C6 C6A C7 C7A . . 172.31(11)
C3A1 C6A C7 C7A . . -7.52(17)
C6 C6A C7 C1P . . -0.83(17)
C3A1 C6A C7 C1P . . 179.33(10)
C6A C7 C7A C8 . . -171.72(10)
C1P C7 C7A C8 . . 1.50(17)
C6A C7 C7A C8A . . 2.04(17)
C1P C7 C7A C8A . . 175.25(10)
C7 C7A C8 C8A . 2_666 168.00(12)
C8A C7A C8 C8A . 2_666 -5.93(19)
C7 C7A C8A C8 . 2_666 -168.40(12)
C8 C7A C8A C8 . 2_666 5.47(18)
C7 C7A C8A C8B . . 8.83(17)
C8 C7A C8A C8B . . -177.30(10)
C2 C1 C8B C3A1 . . -6.23(17)
C1M C1 C8B C3A1 . . 172.20(11)
C2 C1 C8B C8A . . 173.80(11)
C1M C1 C8B C8A . . -7.76(19)
C3A C3A1 C8B C1 . . 8.50(17)
C6A C3A1 C8B C1 . . -171.30(10)
C3A C3A1 C8B C8A . . -171.53(10)
C6A C3A1 C8B C8A . . 8.67(16)
C8 C8A C8B C1 2_666 . -16.91(19)
C7A C8A C8B C1 . . 166.07(11)
C8 C8A C8B C3A1 2_666 . 163.12(11)
C7A C8A C8B C3A1 . . -13.90(16)
C7A C7 C1P C2P . . 81.89(15)
C6A C7 C1P C2P . . -104.89(14)
C7A C7 C1P C6P . . -93.64(14)
C6A C7 C1P C6P . . 79.58(14)
C6P C1P C2P C3P . . 1.16(17)
C7 C1P C2P C3P . . -174.46(10)
C1P C2P C3P C4P . . 0.31(18)
C2P C3P C4P C5P . . -1.40(18)
C2P C3P C4P C1T . . 176.39(11)
C3P C4P C5P C6P . . 1.05(19)
C1T C4P C5P C6P . . -176.83(12)
C4P C5P C6P C1P . . 0.4(2)
C2P C1P C6P C5P . . -1.51(18)
C7 C1P C6P C5P . . 174.24(11)
C3P C4P C1T C3T . . 7.25(18)
C5P C4P C1T C3T . . -175.02(12)
C3P C4P C1T C2T . . -113.67(14)
C5P C4P C1T C2T . . 64.06(15)
C3P C4P C1T C4T . . 127.77(13)
C5P C4P C1T C4T . . -54.50(15)

_cod_database_fobs_code 2241996
