Enantiopure pillar[5]arene active domains within a homochiral metal-organic framework
Nathan L. Strutt; Huacheng Zhang; J. Fraser Stoddart; Chem.Commun. 50 (2014) 7455–; doi:10.1039/C4CC02559H

data_7114637
_publ_section_title
;
 Enantiopure pillar[5]arene active domains within a homochiral
 metal-organic framework
;
_journal_name_full               Chem.Commun.
_journal_page_first              7455
_journal_paper_doi               10.1039/C4CC02559H
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C67 H72 N2 O12, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C67.5 H73 Cl N2 O12'
_chemical_formula_weight         1139.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.817(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0918(5)
_cell_length_b                   21.3853(9)
_cell_length_c                   26.0509(12)
_cell_measurement_reflns_used    4212
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.55
_cell_measurement_theta_min      4.60
_cell_volume                     6728.3(5)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.9
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.899
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10925
_diffrn_reflns_point_group_measured_fraction_full 0.463
_diffrn_reflns_point_group_measured_fraction_max 0.488
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.503
_diffrn_reflns_theta_min         4.467
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.549453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0662 before and 0.0413 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0849 before and 0.0454 after correction.
 The Ratio of minimum to maximum transmission is 0.73.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 38967 reflections, Rint = 0.0797
 (14879 with I > 3sig(I), Rint = 0.0617)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       plate
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.110
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.12(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1500
_refine_ls_number_reflns         10925
_refine_ls_number_restraints     1522
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1895P)^2^+0.3443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2261
_refine_ls_wR_factor_ref         0.2421
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                8786
_reflns_number_total             10925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02559h2.cif
_cod_data_source_block           n2285_sq_s
_cod_depositor_comments
;

2017-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C67 H72 N2 O12), C H2 Cl2'
_cod_original_formula_sum        'C135 H146 Cl2 N4 O24'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2279.45
_cod_database_code               7114637
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.802
_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, All O(H) groups
2. Restrained distances
 O10-C55 \\sim O10A-C55A \\sim O12A-C67A \\sim O12-C67
 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.002
5.a Ternary CH refined with riding coordinates:
 C54(H54), C66(H66), C54A(H54A), C66A(H66A)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C10(H10A,H10B), C19(H19A,H19B), C28(H28A,H28B), C37(H37A,H37B),
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C55(H55A,H55B), C63(H63A,H63B),
  C64(H64A,H64B), C65(H65A,H65B), C67(H67A,H67B), C3A(H3AA,H3AB), C10A(H10D,
 H10E), C19A(H19C,H19D), C28A(H28C,H28D), C37A(H37C,H37D), C51A(H51C,H51D),
 C52A(H52C,H52D), C53A(H53C,H53D), C55A(H55C,H55D), C63A(H63C,H63D), C64A(H64C,
 H64D), C65A(H65C,H65D), C67A(H67C,H67D), C68(H68A,H68B)
5.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C36(H36A,H36B,
 H36C), C18A(H18D,H18E,H18F)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C14(H14), C16(H16), C22(H22), C25(H25), C31(H31), C34(H34),
 C40(H40), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49), C57(H57), C58(H58),
  C60(H60), C61(H61), C1A(H1A), C7A(H7A), C14A(H14A), C16A(H16A), C22A(H22A),
 C25A(H25A), C31A(H31A), C34A(H34A), C40A(H40A), C43A(H43A), C45A(H45A),
 C46A(H46A), C48A(H48A), C49A(H49A), C57A(H57A), C58A(H58A), C60A(H60A),
 C61A(H61A)
5.e Tetrahedral OH refined with riding coordinates:
 O10(H10), O10A(H10C)
5.f Idealised Me refined as rotating group:
 C1B(H1BA,H1BB,H1BC), C9(H9A,H9B,H9C), C26(H26A,H26B,H26C), C35(H35A,H35B,
 H35C), C1AA(H1AA,H1AB,H1AC), C1BA(H1BD,H1BE,H1BF), C9A(H9AA,H9AB,H9AC),
 C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F), C35A(H35D,H35E,H35F), C36A(H36D,
 H36E,H36F)
5.g Idealised tetrahedral OH refined as rotating group:
 O12(H12), O12A(H12A)
;
_shelx_res_checksum              87208
_shelx_fab_checksum              52071