Hydrocarbon Belts with Truncated Cone Structures.
Zhang, Qian; Zhang, Yan-E; Tong, Shuo; Wang, Mei-Xiang; Journal of the American Chemical Society 142 (2020) 1196–1199; doi:10.1021/jacs.9b12181

data_4134122
_publ_section_title
;
 Hydrocarbon Belts with Truncated Cone Structures.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1196
_journal_page_last               1199
_journal_paper_doi               10.1021/jacs.9b12181
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C48 H68'
_chemical_formula_sum            'C48 H68'
_chemical_formula_weight         645.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.119(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5666(4)
_cell_length_b                   11.9458(2)
_cell_length_c                   21.4091(5)
_cell_measurement_reflns_used    44852
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      75.4550
_cell_measurement_theta_min      2.6470
_cell_volume                     4190.89(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -81.00  17.00   0.50    0.05    --  -46.45 102.00 135.00  196
  2  \w    -10.00  81.00   0.50    0.05    --   46.45-102.00  31.00  182
  3  \w   -168.00 -82.00   0.50    0.15    --  -99.00-102.00  31.00  172
  4  \w   -110.00 -26.00   0.50    0.15    --  -99.00 102.00 135.00  168
  5  \w     88.00 169.00   0.50    0.15    --  103.25 102.00 135.00  162
  6  \w     31.00 110.00   0.50    0.15    --  103.25-102.00  31.00  158
  7  \w    -59.00  27.00   0.50    0.05    --  -46.45  38.00  60.00  172
  8  \w   -118.00 -31.00   0.50    0.05    --  -46.45 -57.00 -90.00  174
  9  \w   -118.00 -71.00   0.50    0.05    --  -46.45-125.00-180.00   94
 10  \w   -118.00 -71.00   0.50    0.05    --  -46.45-125.00 150.00   94
 11  \w    -25.00  69.00   0.50    0.05    --   46.45 -77.00-120.00  188
 12  \w     16.00  94.00   0.50    0.05    --   46.45-125.00-150.00  156
 13  \w   -168.00 -85.00   0.50    0.15    --  -99.00 -15.00-120.00  166
 14  \w   -168.00 -86.00   0.50    0.15    --  -99.00 -45.00  60.00  164
 15  \w   -117.00 -26.00   0.50    0.15    --  -99.00 125.00 120.00  182
 16  \w   -112.00 -24.00   0.50    0.15    --  -99.00  30.00 150.00  176
 17  \w   -168.00 -76.00   0.50    0.15    --  -99.00 -77.00 120.00  184
 18  \w   -168.00 -81.00   0.50    0.15    --  -99.00 -94.00   0.00  174
 19  \w   -112.00 -27.00   0.50    0.15    --  -99.00  45.00-120.00  170
 20  \w   -168.00 -85.00   0.50    0.15    --  -99.00 -15.00  90.00  166
 21  \w     31.00 109.00   0.50    0.15    --  103.25 -94.00 -60.00  156
 22  \w     87.00 169.00   0.50    0.15    --  103.25  61.00 -30.00  164
 23  \w     31.00 109.00   0.50    0.15    --  103.25 -94.00-120.00  156
 24  \w     32.00 116.00   0.50    0.15    --  103.25 -45.00 -90.00  168
 25  \w     31.00 120.00   0.50    0.15    --  103.25 -61.00-150.00  178
 26  \w     31.00 117.00   0.50    0.15    --  103.25-125.00  60.00  172
 27  \w     31.00 109.00   0.50    0.15    --  103.25 -94.00-150.00  156
 28  \w     31.00 126.00   0.50    0.15    --  103.25 -77.00  30.00  190
 29  \w     91.00 169.00   0.50    0.15    --  103.25  45.00-180.00  156
 30  \w   -118.00 -24.00   0.50    0.05    --  -46.45 -77.00-180.00  188
 31  \w   -118.00 -72.00   0.50    0.05    --  -46.45 -77.00  90.00   92
 32  \w     24.00 118.00   0.50    0.05    --   46.45  77.00   0.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0902141000
_diffrn_orient_matrix_UB_12      -0.0171544000
_diffrn_orient_matrix_UB_13      -0.0088177000
_diffrn_orient_matrix_UB_21      -0.0193219000
_diffrn_orient_matrix_UB_22      -0.0353771000
_diffrn_orient_matrix_UB_23      -0.0733004000
_diffrn_orient_matrix_UB_31      0.0181956000
_diffrn_orient_matrix_UB_32      -0.1228152000
_diffrn_orient_matrix_UB_33      0.0223817000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            75680
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.735
_diffrn_reflns_theta_min         2.696
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          1.2
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         8529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0829P)^2^+5.5311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8131
_reflns_number_total             8529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12181_si_009.cif
_cod_data_source_block           tx1292a
_cod_original_cell_volume        4190.88(17)
_cod_database_code               4134122
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CH
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C15(H15), C8(H8), C7(H7), C16(H16), C11(H11), C19(H19), C10(H10), C18(H18),
 C27(H27), C39(H39), C33(H33), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C9(H9A,H9B), C44(H44A,H44B), C17(H17A,H17B), C48(H48A,H48B),
 C25(H25A,H25B), C50(H50A,H50B), C41(H41A,H41B), C26(H26A,H26B), C30(H30A,H30B),
  C35(H35A,H35B), C29(H29A,H29B), C45(H45A,H45B), C28(H28A,H28B), C38(H38A,
 H38B), C40(H40A,H40B), C37(H37A,H37B), C34(H34A,H34B), C51(H51A,H51B),
 C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C24(H24), C32(H32), C22(H22)
2.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C43(H43A,H43B,
 H43C)
;
_shelx_res_checksum              35503
_shelx_hkl_checksum              23273
_shelx_fab_checksum              68075
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.282
_oxdiff_exptl_absorpt_empirical_full_min 0.660