<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_4128553
_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         'C2 H3 Cl, C33 H42 O6'
_chemical_formula_sum            'C35 H45 Cl O6'
_chemical_formula_weight         597.16
_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             2019-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3650(3)
_cell_length_b                   13.1318(3)
_cell_length_c                   21.8808(5)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      54.92
_cell_measurement_theta_min      3.42
_cell_volume                     3264.75(14)
_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      111.51
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.0807
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32219
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.948
_diffrn_reflns_theta_min         3.415
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.2015 before and 0.1085 after correction. The Ratio of minimum to maximum transmission is 0.6304. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+2.5112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5129
_reflns_number_total             6170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06188_si_005.cif
_cod_data_source_block           190319zyj_2_0m
_cod_database_code               4128553
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.916
_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 Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C22(H22A,H22B),
 C24(H24A,H24B), C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C4(H4), C7(H7), C11(H11), C14(H14), C18(H18), C21(H21)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              17403
_shelx_hkl_checksum              73689
_olex2_submission_special_instructions 'No special instructions were received'