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_7114638
_publ_section_title
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 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 rm
_chemical_formula_moiety         'C67 H72 N2 O12'
_chemical_formula_sum            'C67 H72 N2 O12'
_chemical_formula_weight         1097.26
_chemical_name_systematic
;
 ?
;
_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                 97.077(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9346(18)
_cell_length_b                   11.7299(11)
_cell_length_c                   21.685(3)
_cell_measurement_reflns_used    2678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.27
_cell_measurement_theta_min      4.11
_cell_volume                     3265.0(7)
_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      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.574
_diffrn_measured_fraction_theta_max 0.967
_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_R_equivalents  0.0939
_diffrn_reflns_av_unetI/netI     0.1417
_diffrn_reflns_Laue_measured_fraction_full 0.574
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12584
_diffrn_reflns_point_group_measured_fraction_full 0.524
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         50.772
_diffrn_reflns_theta_min         4.108
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0856 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission is 0.7641.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 989 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.1(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         6172
_refine_ls_number_restraints     760
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0922
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1450P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2501
_reflns_Friedel_coverage         0.732
_reflns_Friedel_fraction_full    0.468
_reflns_Friedel_fraction_max     0.802
_reflns_number_gt                3457
_reflns_number_total             6172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02559h2.cif
_cod_data_source_block           cu_n2316_0m
_cod_original_cell_volume        3265.1(7)
_cod_database_code               7114638
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.901
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C54(H54), C66(H66)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), 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)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C12(H12A), C15(H15), C21(H21), C24(H24), C30(H30), C33(H33),
 C39(H39), C42(H42), C45(H45), C46(H46), C48(H48), C49(H49), C57(H57), C58(H58),
  C60(H60), C61(H61)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C)
4.e Idealised tetrahedral OH refined as rotating group:
 O10(H10), O12(H12)
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_smtbx_masks_special_details
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The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 637.2 Ang^3^ [19.5%]
Total electron count / cell = 161.2
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_shelx_res_checksum              65250