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_4134121
_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         'C2 H3 O2, C48 H56'
_chemical_formula_sum            'C50 H59 O2'
_chemical_formula_weight         691.97
_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             2019-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.59010(10)
_cell_length_b                   13.8435(2)
_cell_length_c                   26.7612(4)
_cell_measurement_reflns_used    7948
_cell_measurement_temperature    169.99(11)
_cell_measurement_theta_max      73.9530
_cell_measurement_theta_min      3.3150
_cell_volume                     3912.12(9)
_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 0.963
_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    -79.00 -20.00   0.50    0.25    --  -47.45 111.00 166.00  118
  2  \w     16.00  48.00   0.50    0.25    --   47.45-111.00  72.00   64
  3  \w    -93.00 -68.00   0.50    1.50    --  -99.00 111.00 166.00   50
  4  \w   -165.00-134.00   0.50    1.50    --  -99.00-111.00  72.00   62
  5  \w    103.00 128.00   0.50    1.50    --  103.25 111.00 166.00   50
  6  \w     32.00  96.00   0.50    1.50    --  103.25-111.00  72.00  128
  7  \w   -120.00 -73.00   0.50    0.25    --  -47.45-125.00-150.00   94
  8  \w    -24.00  61.00   0.50    0.25    --   47.45 -38.00  30.00  170
  9  \w     34.00 120.00   0.50    0.25    --   47.45  57.00-180.00  172
 10  \w   -168.00 -83.00   0.50    1.50    --  -99.00 -61.00   0.00  170
 11  \w   -148.00 -90.00   0.50    1.50    --  -99.00 -45.00 120.00  116
 12  \w     45.00 106.00   0.50    1.50    --  103.25 -94.00 -30.00  122
 13  \w     34.00  63.00   0.50    1.50    --  103.25 -94.00 -90.00   58
 14  \w    125.00 159.00   0.50    1.50    --  103.25  45.00 -90.00   68
 15  \w     46.00 107.00   0.50    1.50    --  103.25 -94.00-150.00  122
 16  \w     36.00 104.00   0.50    1.50    --  103.25 -94.00 120.00  136
 17  \w     97.00 168.00   0.50    1.50    --  103.25  45.00   0.00  142
 18  \w    121.00 154.00   0.50    1.50    --  103.25  45.00-180.00   66
 19  \w     76.00 103.00   0.50    1.50    --  103.25 -94.00 -90.00   54
;
_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      -0.0665634000
_diffrn_orient_matrix_UB_12      -0.0535578000
_diffrn_orient_matrix_UB_13      -0.0450630000
_diffrn_orient_matrix_UB_21      -0.0076734000
_diffrn_orient_matrix_UB_22      0.0950636000
_diffrn_orient_matrix_UB_23      -0.0300024000
_diffrn_orient_matrix_UB_31      0.1295654000
_diffrn_orient_matrix_UB_32      -0.0218740000
_diffrn_orient_matrix_UB_33      -0.0200697000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            26964
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.376
_diffrn_reflns_theta_min         3.312
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68354
_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    1.175
_exptl_crystal_description       prism
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0791P)^2^+3.5743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1856
_refine_ls_wR_factor_ref         0.2035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5897
_reflns_number_total             7801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12181_si_008.cif
_cod_data_source_block           tx258
_cod_database_code               4134121
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CHNO
_reflns_odcompleteness_completeness 99.97
_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:
 C8(H8), C20(H20), C16(H16), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C35(H35A,H35B), C23(H23A,H23B), C44(H44A,H44B), C50(H50A,
 H50B), C22(H22A,H22B), C41(H41A,H41B), C34(H34A,H34B), C51(H51A,H51B),
 C45(H45A,H45B), C40(H40A,H40B), C48(H48A,H48B), C30(H30A,H30B), C39(H39A,H39B),
  C29(H29A,H29B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C18(H18), C25(H25), C37(H37), C14(H14), C27(H27), C32(H32)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C52(H52A,H52B,H52C), C43(H43A,H43B,H43C), C49(H49A,H49B,
 H49C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              85725
_shelx_hkl_checksum              24615
_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 1.972
_oxdiff_exptl_absorpt_empirical_full_min 0.498