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_4134124
_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         'C66 H60, 4(C4 H5)'
_chemical_formula_sum            'C82 H80'
_chemical_formula_weight         1065.46
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.079(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7064(3)
_cell_length_b                   18.1407(3)
_cell_length_c                   19.7159(4)
_cell_measurement_reflns_used    9724
_cell_measurement_temperature    169.99(11)
_cell_measurement_theta_max      74.1910
_cell_measurement_theta_min      3.3920
_cell_volume                     6020.2(2)
_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(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.957
_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    -69.00  25.00   0.50    0.25    --  -47.45  75.00-149.00  188
  2  \w    -97.00 -72.00   0.50    0.25    --  -47.45 -75.00  83.00   50
  3  \w    -21.00  53.00   0.50    0.25    --   47.45 -75.00  83.00  148
  4  \w     42.00 105.00   0.50    0.25    --   47.45  75.00-149.00  126
  5  \w    -74.00 -39.00   0.50    2.50    --  -99.00  75.00-149.00   70
  6  \w   -168.00-130.00   0.50    2.50    --  -99.00 -75.00  83.00   76
  7  \w    125.00 167.00   0.50    2.50    --  103.25  75.00-149.00   84
  8  \w     38.00 124.00   0.50    2.50    --  103.25 -75.00  83.00  172
  9  \w   -118.00 -71.00   0.50    0.25    --  -47.45-125.00-120.00   94
 10  \w   -168.00 -89.00   0.50    2.50    --  -99.00 -30.00 -90.00  158
 11  \w   -156.00 -87.00   0.50    2.50    --  -99.00 -30.00 -60.00  138
 12  \w   -113.00 -26.00   0.50    2.50    --  -99.00 125.00   0.00  174
 13  \w   -154.00-128.00   0.50    2.50    --  -99.00 -94.00 150.00   52
 14  \w     45.00 116.00   0.50    2.50    --  103.25 -45.00  90.00  142
 15  \w     91.00 169.00   0.50    2.50    --  103.25  30.00-180.00  156
 16  \w     31.00 109.00   0.50    2.50    --  103.25 -94.00 -60.00  156
;
_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      0.0544897000
_diffrn_orient_matrix_UB_12      0.0590572000
_diffrn_orient_matrix_UB_13      -0.0162927000
_diffrn_orient_matrix_UB_21      -0.0078654000
_diffrn_orient_matrix_UB_22      -0.0376056000
_diffrn_orient_matrix_UB_23      -0.0719283000
_diffrn_orient_matrix_UB_31      -0.0730942000
_diffrn_orient_matrix_UB_32      0.0480657000
_diffrn_orient_matrix_UB_33      -0.0362897000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43335
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.560
_diffrn_reflns_theta_min         2.934
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81638
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         11958
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0734
_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^)+(0.1140P)^2^+3.4936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8700
_reflns_number_total             11958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12181_si_006.cif
_cod_data_source_block           tx249
_cod_database_code               4134124
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CH
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.976
_reflns_odcompleteness_completeness 99.87
_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. Restrained distances
 C1-C2
 1.4 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C00C(H00C), C00K(H00K), C013(H013), C016(H016), C01E(H01G), C01I(H01K)
3.b Secondary CH2 refined with riding coordinates:
 C012(H01A,H01B), C01A(H01C,H01D), C01M(H01Q,H01R), C01N(H01S,H01T), C01P(H01X,
 H01Y), C01R(H01,HB)
3.c Aromatic/amide H refined with riding coordinates:
 C004(H004), C00B(H00B), C00E(H00E), C00F(H00F), C00L(H00L), C00M(H00M),
 C00O(H00O), C00Q(H00Q), C00S(H00S), C00T(H00T), C00V(H00V), C00X(H00X),
 C00Y(H00Y), C015(H015), C017(H017), C018(H018), C019(H019), C01B(H01E),
 C01C(H01F), C01F(H01H), C01G(H01I), C01H(H01J), C01J(H01L), C01K(H01M),
 C01V(H3AA), C01W(H4AA), C01Z(H6AA), C020(H020), C022(H022), C023(H023),
 C025(H025), C2(H2)
3.d Idealised Me refined as rotating group:
 C01L(H01N,H01O,H01P), C01O(H01U,H01V,H01W), C01Q(H01Z,H,HA), C01S(H0AA,HC,HD),
  C01T(H1AA,HE,HF), C01U(H2AA,HG,HH), C01Y(H5AA,HI,HJ), C3(H3A,H3B,H3C), C4(H4A,
 H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              2436
_shelx_hkl_checksum              98094
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.812