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_4134240
_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         '2(C H2 Cl), C76 H80'
_chemical_formula_sum            'C78 H84 Cl2'
_chemical_formula_weight         1092.35
_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     dual
_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                78.101(2)
_cell_angle_beta                 71.786(2)
_cell_angle_gamma                84.391(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1391(3)
_cell_length_b                   15.2551(4)
_cell_length_c                   15.3506(3)
_cell_measurement_reflns_used    12777
_cell_measurement_temperature    105.4(5)
_cell_measurement_theta_max      71.3820
_cell_measurement_theta_min      4.3310
_cell_volume                     3075.57(13)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105.4(5)
_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 0.973
_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   -109.00 -17.00   1.00    1.00    --  -40.81 -57.00 -30.00   92
  2  \w    -69.00  30.00   1.00    1.00    --  -40.81  57.00 120.00   99
  3  \w    -85.00  -7.00   1.00    1.00    --  -40.81 125.00-180.00   78
  4  \w     22.00 111.00   1.00    1.00    --   40.81  38.00-120.00   89
  5  \w    114.00 150.00   1.00    1.00    --  100.91 125.00-180.00   36
  6  \w    121.00 154.00   1.00    1.00    --  100.91  61.00-120.00   33
  7  \w     27.00 106.00   1.00    1.00    --  100.91 -77.00  90.00   79
  8  \w     33.00 113.00   1.00    1.00    --  100.91 -45.00-180.00   80
  9  \w     60.00 100.00   1.00    1.00    --  100.91 -95.00  30.00   40
 10  \w     28.00 116.00   1.00    1.00    --  100.91 -45.00  90.00   88
 11  \w     69.00 110.00   1.00    1.00    --  100.91 -95.00-180.00   41
 12  \w     19.00 109.00   1.00    1.00    --  100.91 -95.00 -60.00   90
 13  \w     93.00 118.00   1.00    1.00    --  100.91-125.00-180.00   25
 14  \w     33.00 123.00   1.00    1.00    --  100.91 -45.00 -90.00   90
 15  \w     13.00 171.00   1.00    1.00    --  100.91   0.00  60.00  158
;
_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      -0.0218714000
_diffrn_orient_matrix_UB_12      -0.0972071000
_diffrn_orient_matrix_UB_13      0.0009023000
_diffrn_orient_matrix_UB_21      0.1041361000
_diffrn_orient_matrix_UB_22      -0.0107952000
_diffrn_orient_matrix_UB_23      -0.0693471000
_diffrn_orient_matrix_UB_31      0.0430276000
_diffrn_orient_matrix_UB_32      -0.0331509000
_diffrn_orient_matrix_UB_33      0.0821679000
_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  0.0268
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21957
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.435
_diffrn_reflns_theta_min         3.777
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88484
_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    1.180
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         11645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0650P)^2^+1.9305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10345
_reflns_number_total             11645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00112_si_008.cif
_cod_data_source_block           sth-179-1-dce-meoh
_cod_database_code               4134240
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.96
_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:
 C6(H6), C3(H3), C65(H65), C25(H25), C22(H22), C42(H42), C46(H46), C62(H62),
 C53(H53), C35(H35), C74(H74), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C56(H56A,H56B), C26(H26A,H26B), C66(H66A,H66B), C77(H77A,H77B),
 C025(H02A,H02B)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C00H(H00H), C61(H61), C58(H58), C41(H41), C21(H21), C00O(H00O),
 C38(H38), C29(H29), C10(H10), C48(H48), C69(H69), C51(H51), C49(H49), C50(H50),
  C11(H11), C70(H70), C31(H31), C33(H33), C72(H72), C71(H71), C32(H32),
 C12(H12), C13(H13)
2.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C1(H1A,H1B,H1C), C67(H67A,H67B,H67C), C57(H57A,H57B,
 H57C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C37(H37A,H37B,H37C), C36(H36A,
 H36B,H36C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C76(H76A,H76B,H76C),
 C75(H75A,H75B,H75C)
;
_shelx_res_checksum              7913
_shelx_hkl_checksum              567
_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 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.756