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_4134120
_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
'C0.91 H2 Cl1.5, C0.65 H1.29 Cl1.15, C66 H58, Cl'
_chemical_formula_sum            'C67.53 H61.29 Cl3.64'
_chemical_formula_weight         1002.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 112.475(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.0129(12)
_cell_length_b                   14.4043(5)
_cell_length_c                   25.2944(10)
_cell_measurement_reflns_used    4277
_cell_measurement_temperature    100.2(9)
_cell_measurement_theta_max      70.7380
_cell_measurement_theta_min      3.7880
_cell_volume                     11114.6(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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      100.2(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.968
_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    -62.00  27.00   1.00   11.00    --  -40.81  38.00 150.00   89
  2  \w      1.00  61.00   1.00   11.00    --   40.81 -99.00 -60.00   60
  3  \w     24.00  51.00   1.00   11.00    --   40.81-125.00  60.00   27
  4  \w     58.00  97.00   1.00   11.00    --   40.81-125.00 150.00   39
  5  \w     30.00  73.00   1.00    9.42    --  100.91 -45.00 -60.00   43
  6  \w     87.00 120.00   1.00    9.42    --  100.91 -45.00 -60.00   33
  7  \w     81.00 177.00   1.00    9.42    --  100.91  77.00 150.00   96
  8  \w     78.00 105.00   1.00    9.42    --  100.91  45.00-150.00   27
  9  \w     94.00 174.00   1.00    9.42    --  100.91 125.00 -90.00   80
 10  \w    113.00 144.00   1.00    9.42    --  100.91  45.00-150.00   31
 11  \w     80.00 173.00   1.00    9.42    --  100.91  61.00  90.00   93
 12  \w    117.00 142.00   1.00    9.42    --  100.91 125.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0226874000
_diffrn_orient_matrix_UB_12      -0.0805941000
_diffrn_orient_matrix_UB_13      0.0405539000
_diffrn_orient_matrix_UB_21      0.0339307000
_diffrn_orient_matrix_UB_22      -0.0073449000
_diffrn_orient_matrix_UB_23      -0.0280101000
_diffrn_orient_matrix_UB_31      0.0297427000
_diffrn_orient_matrix_UB_32      0.0699166000
_diffrn_orient_matrix_UB_33      0.0437441000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21676
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.514
_diffrn_reflns_theta_min         3.605
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       prism
_exptl_crystal_F_000             4228
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.948
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.294
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         10490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.294
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.1151
_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          0.3206
_refine_ls_wR_factor_ref         0.3593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7316
_reflns_number_total             10490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12181_si_005.cif
_cod_data_source_block           exp_2404
_cod_original_cell_volume        11114.6(7)
_cod_database_code               4134120
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CH
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.931
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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(Cl1)=Sof(C22)=Sof(H22A)=Sof(H22B)=FVAR(1)
 Fixed Sof: Cl2(0.5) Cl3(0.5) Cl3A(0.5) Cl2A(0.5)
3.a Ternary CH refined with riding coordinates:
 C00A(H00C), C00J(H00J), C01B(H01E), C01G(H01I), C01N(H01Q), C01Q(H01U)
3.b Secondary CH2 refined with riding coordinates:
 C008(H00A,H00B), C01J(H01K,H01L), C01K(H01M,H01N), C01L(H01O,H01P), C01O(H01R,
 H01S), C01V(H01,HC), C22(H22A,H22B), C23(H23A,H23B)
3.c Aromatic/amide H refined with riding coordinates:
 C007(H007), C00D(H00D), C00L(H00L), C00N(H00N), C00R(H00R), C00S(H00S),
 C00U(H00U), C00V(H00V), C00Z(H00Z), C011(H011), C012(H012), C013(H013),
 C015(H015), C016(H016), C01A(H01D), C01C(H01F), C01E(H01G), C01F(H01H),
 C01H(H01J), C01P(H01T), C01R(H01V), C01S(H01W)
3.d Idealised Me refined as rotating group:
 C018(H01A,H01B,H01C), C01T(H01X,H01Y,H), C01U(H01Z,HA,HB), C01W(H0AA,HD,HE),
 C01X(H1AA,HF,HG), C01Z(H2AA,HH,HI)
;
_shelx_res_checksum              90187
_shelx_hkl_checksum              25868
_shelx_fab_checksum              21492
_olex2_date_sample_data_collection 2018-05-16
_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 2.542
_oxdiff_exptl_absorpt_empirical_full_min 0.587