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_4134125
_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         '2(C H Cl3), 2(C48 H48)'
_chemical_formula_sum            'C98 H98 Cl6'
_chemical_formula_weight         1488.46
_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             2019-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.643(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4244(5)
_cell_length_b                   10.1229(2)
_cell_length_c                   42.5630(10)
_cell_measurement_reflns_used    10663
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      73.9620
_cell_measurement_theta_min      4.1990
_cell_volume                     7826.2(3)
_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      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_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    -24.00  63.00   0.50    0.05    --   47.07 -60.00  15.00  174
  2  \w     32.00 119.00   0.50    0.05    --  103.25 -60.00  15.00  174
  3  \w     91.00 169.00   0.50    0.05    --  103.25  30.00 120.00  156
  4  \w     87.00 169.00   0.50    0.05    --  103.25  60.00 155.00  164
  5  \w     31.00 119.00   0.50    0.05    --   47.07  60.00 155.00  176
  6  \w     25.00 119.00   0.50    0.05    --   47.07  77.00 -30.00  188
  7  \w     28.00 116.00   0.50    0.05    --  103.25 -30.00-180.00  176
  8  \w     31.00 109.00   0.50    0.05    --  103.25 -94.00   0.00  156
  9  \w     31.00 109.00   0.50    0.05    --  103.25 -94.00 -30.00  156
 10  \w     32.00 116.00   0.50    0.05    --  103.25 -45.00 -60.00  168
 11  \w     31.00 109.00   0.50    0.05    --  103.25 -94.00-150.00  156
 12  \w     31.00 109.00   0.50    0.05    --  103.25 -94.00 -60.00  156
 13  \w     16.00  95.00   0.50    0.05    --   47.07-125.00 -90.00  158
 14  \w     25.00 119.00   0.50    0.05    --   47.07  77.00-120.00  188
 15  \w     25.00 119.00   0.50    0.05    --   47.07  77.00  60.00  188
 16  \w    -63.00  25.00   0.50    0.05    --  -47.07  60.00 155.00  176
 17  \w    -60.00  28.00   0.50    0.05    --  -47.07  19.00 150.00  176
 18  \w   -119.00 -31.00   0.50    0.05    --  -47.07 -60.00  15.00  176
 19  \w   -112.00 -24.00   0.50    0.05    --  -99.00  30.00 150.00  176
 20  \w   -115.00 -27.00   0.50    0.05    --  -99.00  60.00 155.00  176
 21  \w   -122.00 -26.00   0.50    0.05    --  -99.00  77.00 150.00  192
 22  \w   -115.00 -26.00   0.50    0.05    --  -99.00  61.00 -30.00  178
 23  \w   -117.00 -26.00   0.50    0.05    --  -99.00 125.00 120.00  182
 24  \w   -117.00 -26.00   0.50    0.05    --  -99.00 125.00 150.00  182
 25  \w   -117.00 -26.00   0.50    0.05    --  -99.00 125.00 -30.00  182
 26  \w   -168.00 -83.00   0.50    0.05    --  -99.00 -60.00  15.00  170
 27  \w   -119.00 -71.00   0.50    0.05    --  -47.07-125.00 -60.00   96
 28  \w   -119.00 -71.00   0.50    0.05    --  -47.07-125.00-180.00   96
 29  \w   -168.00 -86.00   0.50    0.05    --  -99.00 -45.00 -30.00  164
 30  \w   -168.00 -85.00   0.50    0.05    --  -99.00 -15.00-150.00  166
 31  \w   -168.00 -81.00   0.50    0.05    --  -99.00 -94.00  90.00  174
;
_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      0.0723227000
_diffrn_orient_matrix_UB_12      0.0731658000
_diffrn_orient_matrix_UB_13      -0.0021153000
_diffrn_orient_matrix_UB_21      -0.0415345000
_diffrn_orient_matrix_UB_22      0.0914985000
_diffrn_orient_matrix_UB_23      -0.0258813000
_diffrn_orient_matrix_UB_31      -0.0153695000
_diffrn_orient_matrix_UB_32      0.0971357000
_diffrn_orient_matrix_UB_33      0.0259625000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1473
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            144182
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.634
_diffrn_reflns_theta_min         2.106
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48249
_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    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.396
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.421
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         15873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.421
_refine_ls_R_factor_all          0.1845
_refine_ls_R_factor_gt           0.1406
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3849
_refine_ls_wR_factor_ref         0.4208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8572
_reflns_number_total             15873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12181_si_002.cif
_cod_data_source_block           tx211
_cod_database_code               4134125
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CH
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.649
_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. Others
 Sof(Cl1A)=Sof(Cl2A)=Sof(Cl)=Sof(C02X)=Sof(H9AA)=1-FVAR(1)
 Sof(Cl03)=Sof(Cl1)=Sof(Cl2)=Sof(C02W)=Sof(H8AA)=FVAR(1)
 Sof(Cl3)=Sof(C0AA)=Sof(H0AB)=Sof(Cl4)=Sof(Cl5)=1-FVAR(2)
 Sof(Cl01)=Sof(Cl02)=Sof(Cl00)=Sof(C02V)=Sof(H7AA)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C00L(H00L), C00M(H00M), C00Q(H00Q), C00S(H00S), C00V(H00V), C00W(H00W),
 C015(H015), C01C(H01N), C02V(H7AA), C02W(H8AA), C02X(H9AA), C0AA(H0AB)
3.b Secondary CH2 refined with riding coordinates:
 C00E(H00A,H00B), C00K(H00C,H00E), C00O(H00H,H00I), C010(H01A,H01B), C012(H01C,
 H01D), C016(H01J,H01K), C017(H01L,H01M), C018(H01E,H01F), C01N(H01U,H01V),
 C01V(H01Y,H), C01Y(H01H,H01I), C020(H02A,H02B), C026(H02V,H02W), C02G(H02G,
 H02H), C02K(H0AA,HC), C02S(H6AA,HJ)
3.c Aromatic/amide H refined with riding coordinates:
 C007(H007), C009(H009), C00A(H00G), C00D(H00D), C00F(H00F), C00J(H00J),
 C00P(H00P), C00Z(H00Z), C014(H014), C01E(H01G), C01F(H01Q), C01I(H01R),
 C01L(H01S), C01M(H01T), C01O(H01O), C01P(H01P), C01R(H01W), C01X(H01X),
 C024(H024), C025(H025), C027(H027), C029(H029), C02A(H02X), C02B(H02C),
 C02D(H02D), C02E(H02E), C02F(H02F), C02H(H02Z), C02I(H02I), C02J(H02),
 C02L(H1AA), C02M(H2AA)
3.d Idealised Me refined as rotating group:
 C02C(H02Y,HA,HB), C02N(H3AA,HD,HE), C02O(H02J,H02K,H02L), C02P(H02M,H02N,
 H02O), C02Q(H4AA,HF,HG), C02R(H5AA,HH,HI), C02T(H02P,H02Q,H02R), C02U(H02S,
 H02T,H02U)
;
_shelx_res_checksum              594
_shelx_hkl_checksum              90209
_shelx_fab_checksum              52246
_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 2.026
_oxdiff_exptl_absorpt_empirical_full_min 0.563