Functionalised cyclodextrin-based metal-organic frameworks
Hartlieb, Karel J.; Peters, Aaron William; Wang, Timothy C.; Deria, Pravas; Farha, Omar; Hupp, J. T.; Stoddart, J. Fraser; Chem. Commun.  (2017) –; doi:10.1039/C7CC03345A

data_7120272
_publ_section_title
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 Functionalised cyclodextrin-based metal-organic frameworks
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03345A
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C56 H83 N O41, 2(H2 O)'
_chemical_formula_sum            'C56 H87 N O43'
_chemical_formula_weight         1462.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2015-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-01-05 deposited with the CCDC.
2017-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9905(8)
_cell_length_b                   16.4042(11)
_cell_length_c                   37.700(3)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.796
_cell_measurement_theta_min      2.938
_cell_volume                     7415.4(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.91
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            60413
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.311
_diffrn_reflns_theta_min         3.572
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  0.6682
_exptl_absorpt_correction_T_min  0.5930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0687 after correction.
The Ratio of minimum to maximum transmission is 0.8875.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 4504 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         13418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0820
_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^)+(0.1710P)^2^+2.1820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2317
_refine_ls_wR_factor_ref         0.2397
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                11379
_reflns_number_total             13418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03345a2.cif
_cod_data_source_block           cx0359
_cod_original_cell_volume        7415.3(9)
_cod_database_code               7120272
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.912
_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 O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C5(H5A), C7(H7), C8(H8A), C9(H9A),
 C10(H10A), C11(H11), C13(H13A), C14(H14A), C15(H15A), C16(H16), C17(H17),
 C19(H19A), C20(H20A), C21(H21), C22(H22), C23(H23A), C25(H25A), C26(H26),
 C27(H27), C28(H28A), C29(H29A), C31(H31), C32(H32), C33(H33A), C34(H34A),
 C35(H35A), C37(H37), C38(H38A), C39(H39A), C40(H40), C41(H41), C43(H43),
 C44(H44), C45(H45), C46(H46), C47(H47)
2.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B),
 C36(H36A,H36B), C42(H42A,H42B), C48(H48A,H48B)
2.d Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C53(H53), C54(H54)
2.e Tetrahedral OH refined with riding coordinates:
 O9(H9), O14(H14), O18(H18), O35(H35)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O5(H5), O8(H8), O10(H10), O13(H13), O15(H15), O19(H19),
 O20(H20), O23(H23), O24(H24), O25(H25), O28(H28), O29(H29), O30(H30), O33(H33),
  O34(H34), O38(H38), O39(H39)
;
_smtbx_masks_special_details
;
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 = 1432.9 Ang^3^ [19.3%]
Total electron count / cell = 280.2
;
_shelx_res_checksum              38826
_olex2_date_sample_data_collection 2015-03-27
_olex2_date_sample_submission    2015-03-20
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in oil'
_olex2_submission_original_sample_id KJH_4-142
_olex2_submission_special_instructions 'No special instructions were received'