<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_4128555
_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         'C66 H84 O12, 3(C4 Cl)'
_chemical_formula_sum            'C78 H102 Cl3 O12'
_chemical_formula_weight         1337.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 120.301(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.441(4)
_cell_length_b                   12.5644(18)
_cell_length_c                   25.776(4)
_cell_measurement_reflns_used    4666
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      54.977
_cell_measurement_theta_min      3.333
_cell_volume                     7393(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.968
_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_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7058
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.842
_diffrn_reflns_theta_min         3.369
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 95693 reflections, Rint = 0.0603
 (68649 with I > 3sig(I), Rint = 0.0581)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.370
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7058
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.1292
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+70.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2839
_refine_ls_wR_factor_ref         0.2869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6298
_reflns_number_total             7058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06188_si_004.cif
_cod_data_source_block           190319zyj_3_0m
_cod_database_code               4128555
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.550(3)
 0.450(3)
2. 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
3. Restrained distances
 C38-C39 = C37-C38
 1.5 with sigma of 0.02
 C42-C40_$1
 1.5 with sigma of 0.02
 C34-C35
 1.5 with sigma of 0.02
 C36-C35
 1.5 with sigma of 0.02
 Cl1-C35
 2.8 with sigma of 0.02
 Cl1_$1-C36
 2.5 with sigma of 0.02
 C40-C41
 1.5 with sigma of 0.02
 C41-C42
 1.3 with sigma of 0.02
 Cl1_$1-C34_$1
 1.8 with sigma of 0.02
 C36-C34_$1
 1.5 with sigma of 0.02
 C36-C36_$1
 2.4 with sigma of 0.02
 Cl3-C40
 1.8 with sigma of 0.02
 Cl2-C37 = Cl2-C39
 2.5 with sigma of 0.02
 Cl3-C41
 2.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim C37 \\sim C38 \\sim C39: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Cl3 \\sim C40 \\sim C41 \\sim C42: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Cl1 \\sim C34 \\sim C35 \\sim C36: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C40 \\sim Cl3 \\sim C41 \\sim C42: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(Cl1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Cl2(0.5) C37(0.5) C39(0.5) Cl1(0.5) C35(0.5) C36(0.5) Cl3(0.5)
 C41(0.5) C42(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B),
 C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C13(H13), C17(H17), C20(H20)
6.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              21222
_shelx_hkl_checksum              72097
_olex2_submission_special_instructions 'No special instructions were received'