Toward the synthesis of a highly strained hydrocarbon belt.
Shi, Tan-Hao; Guo, Qing-Hui; Tong, Shuo; Wang, Mei-Xiang; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00112

data_4134247
_publ_section_title
;
 Toward the synthesis of a highly strained hydrocarbon belt.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00112
_journal_year                    2020
_chemical_formula_moiety         'C104 H64 Cl8 N8 O8'
_chemical_formula_sum            'C104 H64 Cl8 N8 O8'
_chemical_formula_weight         1837.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-11-23
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                99.833(4)
_cell_angle_beta                 96.296(5)
_cell_angle_gamma                101.675(5)
_cell_formula_units_Z            2
_cell_length_a                   14.0137(10)
_cell_length_b                   14.8522(7)
_cell_length_c                   30.5015(14)
_cell_measurement_reflns_used    8886
_cell_measurement_temperature    102(1)
_cell_measurement_theta_max      71.7340
_cell_measurement_theta_min      3.6860
_cell_volume                     6056.9(6)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 n/a (Burla et al.,  2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102(1)
_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 0.963
_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   -111.00 -16.00   1.00    6.63    --  -40.31 -57.00 -90.00   95
  2  \w    -66.00  33.00   1.00    6.63    --  -40.31  57.00  60.00   99
  3  \w    -65.00  34.00   1.00    6.63    --  -40.31  38.00-150.00   99
  4  \w     57.00  87.00   1.00    6.63    --   40.31-125.00-150.00   30
  5  \w    112.00 173.00   1.00   26.52    --  100.91  61.00-180.00   61
  6  \w     58.00 110.00   1.00   26.52    --  100.91 -95.00 -30.00   52
  7  \w     26.00 115.00   1.00   26.52    --  100.91 -77.00  30.00   89
  8  \w     29.00 112.00   1.00   26.52    --  100.91 -45.00  30.00   83
  9  \w     28.00 113.00   1.00   26.52    --  100.91 -45.00 120.00   85
 10  \w    112.00 157.00   1.00   26.52    --  100.91 125.00 120.00   45
 11  \w     67.00  99.00   1.00   26.52    --  100.91-125.00-150.00   32
 12  \w     19.00 108.00   1.00   26.52    --  100.91 -95.00-120.00   89
 13  \w     34.00 123.00   1.00   26.52    --  100.91 -45.00-150.00   89
 14  \w     93.00 118.00   1.00   26.52    --  100.91-125.00-180.00   25
 15  \w     13.00 164.00   1.00   26.52    --  100.91   0.00-180.00  151
;
_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      -0.0441474000
_diffrn_orient_matrix_UB_12      -0.0990857000
_diffrn_orient_matrix_UB_13      -0.0282763000
_diffrn_orient_matrix_UB_21      -0.0937577000
_diffrn_orient_matrix_UB_22      0.0316176000
_diffrn_orient_matrix_UB_23      -0.0160384000
_diffrn_orient_matrix_UB_31      0.0463631000
_diffrn_orient_matrix_UB_32      0.0293216000
_diffrn_orient_matrix_UB_33      -0.0403847000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            41401
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.732
_diffrn_reflns_theta_min         3.695
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60600
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.007
_exptl_crystal_description       plate
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.549
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.325
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         22843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_all          0.1601
_refine_ls_R_factor_gt           0.1318
_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          0.3647
_refine_ls_wR_factor_ref         0.3834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14907
_reflns_number_total             22843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00112_si_014.cif
_cod_data_source_block           sth-318-2_sqd
_cod_database_code               4134247
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.489
_reflns_odcompleteness_completeness 99.86
_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:
 C83(H83), C53(H53), C29(H29), C9(H9), C56(H56), C32(H32), C80(H80), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C95(H95A,H95B), C19(H19A,H19B), C69(H69A,H69B), C45(H45A,H45B)
2.c Aromatic/amide H refined with riding coordinates:
 C72(H72), C22(H22), C52(H52), C26(H26), C102(H102), C76(H76), C48(H48),
 C50(H50), C79(H79), C98(H98), C100(H100), C24(H24)
2.d Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C70(H70A,H70B,
 H70C), C78(H78A,H78B,H78C), C105(H10A,H10B,H10C), C106(H10D,H10E,H10F),
 C96(H96A,H96B,H96C), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C46(H46A,H46B,
 H46C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              75657
_shelx_hkl_checksum              16694
_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 1.775
_oxdiff_exptl_absorpt_empirical_full_min 0.683
_platon_squeeze_void_probe_radius 1.20