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_4134123
_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 H56, C2 H3 N'
_chemical_formula_sum            'C50 H59 N'
_chemical_formula_weight         673.98
_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             2019-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1678(2)
_cell_length_b                   17.2717(3)
_cell_length_c                   17.8226(2)
_cell_measurement_reflns_used    10700
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.0550
_cell_measurement_theta_min      3.5550
_cell_volume                     4319.69(11)
_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      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.966
_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   -123.00 -34.00   0.50    0.05    --  -47.20 -18.00-174.00  178
  2  \w    -40.00 -15.00   0.50    0.05    --  -47.20  18.00  -5.00   50
  3  \w     34.00  91.00   0.50    0.05    --   47.20  18.00  -5.00  114
  4  \w    -13.00  47.00   0.50    0.05    --   47.20 -18.00-174.00  120
  5  \w    -92.00 -67.00   0.50    0.08    --  -99.00  18.00  -5.00   50
  6  \w   -137.00 -86.00   0.50    0.08    --  -99.00 -18.00-174.00  102
  7  \w     29.00 104.00   0.50    0.08    --  103.25 -18.00-174.00  150
  8  \w     90.00 169.00   0.50    0.08    --  103.25  18.00  -5.00  158
  9  \w     17.00  93.00   0.50    0.05    --   47.20-125.00  90.00  152
 10  \w   -111.00 -28.00   0.50    0.08    --  -99.00  45.00-150.00  166
 11  \w    -60.00 -26.00   0.50    0.08    --  -99.00 125.00  30.00   68
 12  \w   -103.00 -66.00   0.50    0.08    --  -99.00 125.00  30.00   74
 13  \w     35.00 115.00   0.50    0.08    --  103.25 -30.00  60.00  160
 14  \w    111.00 136.00   0.50    0.08    --  103.25  45.00-150.00   50
 15  \w     70.00  96.00   0.50    0.08    --  103.25 -94.00-180.00   52
 16  \w     43.00 114.00   0.50    0.08    --  103.25 -30.00 -30.00  142
 17  \w     31.00  93.00   0.50    0.08    --  103.25 -94.00-120.00  124
 18  \w     63.00 109.00   0.50    0.08    --  103.25 -94.00 150.00   92
;
_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      0.0702380000
_diffrn_orient_matrix_UB_12      -0.0003039000
_diffrn_orient_matrix_UB_13      0.0741081000
_diffrn_orient_matrix_UB_21      -0.0819454000
_diffrn_orient_matrix_UB_22      -0.0214511000
_diffrn_orient_matrix_UB_23      0.0446781000
_diffrn_orient_matrix_UB_31      0.0200337000
_diffrn_orient_matrix_UB_32      -0.0865806000
_diffrn_orient_matrix_UB_33      -0.0113317000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31399
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.314
_diffrn_reflns_theta_min         3.580
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63178
_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    1.036
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         8635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1024P)^2^+1.3923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.1885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6567
_reflns_number_total             8635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12181_si_007.cif
_cod_data_source_block           exp_61
_cod_database_code               4134123
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         chn
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.845
_reflns_odcompleteness_completeness 99.98
_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:
 C17(H17), C5(H5), C13(H13), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C37(H37A,H37B), C44(H44A,H44B), C38(H38A,H38B), C19(H19A,
 H19B), C48(H48A,H48B), C20(H20A,H20B), C41(H41A,H41B), C27(H27A,H27B),
 C36(H36A,H36B), C31(H31A,H31B), C26(H26A,H26B), C45(H45A,H45B), C39(H39A,H39B),
  C42(H42A,H42B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C22(H22), C7(H7), C15(H15), C11(H11), C24(H24), C29(H29), C34(H34)
2.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C57(H57A,H57B,H57C), C40(H40A,H40B,H40C), C46(H46A,H46B,
 H46C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              32793
_shelx_hkl_checksum              23773
_shelx_fab_checksum              70635
_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 1.688
_oxdiff_exptl_absorpt_empirical_full_min 0.627