<i>Cis</i>-<i>Trans</i> Selectivity of Haloalkene Isomers in Nonporous Adaptive Pillararene Crystals.
Zhou, Yujuan; Jie, Kecheng; Zhao, Run; Huang, Feihe; Journal of the American Chemical Society 141 (2019) 11847–11851; doi:10.1021/jacs.9b06188

data_4128554
_publ_section_title
;
 <i>Cis</i>-<i>Trans</i> Selectivity of Haloalkene Isomers in Nonporous
 Adaptive Pillararene Crystals.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11847
_journal_page_last               11851
_journal_paper_doi               10.1021/jacs.9b06188
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C4 H6 Cl2, C55 H70 O10'
_chemical_formula_sum            'C59 H76 Cl2 O10'
_chemical_formula_weight         1016.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.026(2)
_cell_length_b                   15.8064(8)
_cell_length_c                   16.2928(8)
_cell_measurement_reflns_used    9515
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      52.752
_cell_measurement_theta_min      7.559
_cell_volume                     11080.5(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66299
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.884
_diffrn_reflns_theta_min         3.505
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1377 before and 0.0657 after correction. The Ratio of minimum to maximum transmission is 0.6918. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10510
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+12.7398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7265
_reflns_number_total             10510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06188_si_003.cif
_cod_data_source_block           190423zyj_2
_cod_original_cell_volume        11080.6(9)
_cod_database_code               4128554
_shelx_shelxl_version_number     2016/6
_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. Restrained distances
 C3-C2
 1.3 with sigma of 0.01
 C33-C32
 1.53 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C9(H9A,H9B), C13(H13A,H13B), C16(H16A,H16B),
 C21(H21A,H21B), C24(H24A,H24B), C27(H27A,H27B), C32(H32A,H32B), C35(H35A,H35B),
  C38(H38A,H38B), C43(H43A,H43B), C46(H46A,H46B), C49(H49A,H49B), C54(H54A,
 H54B), C57(H57A,H57B), C58(H58A,H58B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C12(H12), C18(H18), C23(H23), C29(H29), C34(H34),
 C40(H40), C45(H45), C51(H51), C56(H56)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C28(H28A,H28B,
 H28C), C33(H33A,H33B,H33C), C39(H39A,H39B,H39C), C44(H44A,H44B,H44C), C50(H50A,
 H50B,H50C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              63542
_shelx_hkl_checksum              68706
_olex2_submission_special_instructions 'No special instructions were received'