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_4134119
_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 H48, C2 H3 N, C H Cl3'
_chemical_formula_sum            'C51 H52 Cl3 N'
_chemical_formula_weight         785.33
_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     direct
_audit_creation_date             2018-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.972(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2903(5)
_cell_length_b                   17.0847(4)
_cell_length_c                   17.5892(5)
_cell_measurement_reflns_used    3660
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.0600
_cell_measurement_theta_min      4.5160
_cell_volume                     4252.8(2)
_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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_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    -61.00  29.00   1.00    8.00    --  -40.81  38.00-180.00   90
  2  \w   -112.00 -25.00   1.00    8.00    --  -40.81 -57.00-150.00   87
  3  \w     35.00  78.00   1.00    8.00    --   40.81 -99.00-150.00   43
  4  \w     28.00  57.00   1.00   18.00    --  100.91 -30.00-150.00   29
  5  \w     46.00 113.00   1.00   18.00    --  100.91-125.00  90.00   67
  6  \w     93.00 156.00   1.00   18.00    --  100.91  45.00 -60.00   63
  7  \w     83.00 121.00   1.00   18.00    --  100.91 -30.00-150.00   38
  8  \w     25.00 122.00   1.00   18.00    --  100.91 -30.00 120.00   97
  9  \w     27.00 119.00   1.00   18.00    --  100.91 -77.00  90.00   92
;
_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      -0.0755111000
_diffrn_orient_matrix_UB_12      -0.0063220000
_diffrn_orient_matrix_UB_13      0.0542161000
_diffrn_orient_matrix_UB_21      -0.0776521000
_diffrn_orient_matrix_UB_22      -0.0056347000
_diffrn_orient_matrix_UB_23      -0.0699302000
_diffrn_orient_matrix_UB_31      0.0103750000
_diffrn_orient_matrix_UB_32      -0.0897747000
_diffrn_orient_matrix_UB_33      0.0005245000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15651
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.460
_diffrn_reflns_theta_min         3.624
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93261
_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 light colourless'
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.705
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.471
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.471
_refine_ls_R_factor_all          0.1603
_refine_ls_R_factor_gt           0.1252
_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          0.3612
_refine_ls_wR_factor_ref         0.3981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5417
_reflns_number_total             8028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12181_si_003.cif
_cod_data_source_block           exp_3520
_cod_depositor_comments
;

2020-08-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '0.03(C48 H48), 0.03(C2 H3 N), 0.03(C H Cl3)'
_cod_original_formula_sum        'C1.71 H1.75 Cl0.10 N0.03'
_cod_original_formula_units_Z    119
_cod_original_formula_weight     26.40
_cod_database_code               4134119
_chemical_oxdiff_formula         CHN
_reflns_odcompleteness_completeness 99.89
_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.a Ternary CH refined with riding coordinates:
 C00C(H00C), C00S(H00S), C00Z(H00Z), C012(H012), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C00E(H00B,H00D), C00Y(H00E,H00F), C011(H01A,H01B), C014(H01C,H01D), C017(H01E,
 H01F), C01A(H01G,H01H), C01D(H01L,H01M), C01H(H01T,H01U)
2.c Aromatic/amide H refined with riding coordinates:
 C005(H005), C008(H008), C00A(H00A), C00G(H00G), C00M(H00M), C00N(H00N),
 C00P(H00P), C00Q(H00Q), C00T(H00T), C00U(H00U), C00W(H00W), C00X(H00X),
 C013(H013), C015(H015), C016(H016), C018(H018)
2.d Idealised Me refined as rotating group:
 C019(H01Y,H,HA), C01C(H01I,H01J,H01K), C01E(H01N,H01O,H01P), C01G(H01Q,H01R,
 H01S), C01I(H01V,H01W,H01X)
;
_shelx_res_checksum              34882
_shelx_hkl_checksum              83029
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2018-12-06
_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 1.285
_oxdiff_exptl_absorpt_empirical_full_min 0.702