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_7120271
_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         'C48 H81 N O39 Rb2'
_chemical_formula_sum            'C48 H81 N O39 Rb2'
_chemical_formula_weight         1467.07
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_Hall           'I 4 2 3'
_space_group_name_H-M_alt        'I 4 3 2'
_symmetry_space_group_name_Hall  'I 4 2 3'
_symmetry_space_group_name_H-M   'I 4 3 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2015-04-02
_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            12
_cell_length_a                   31.0197(11)
_cell_length_b                   31.0197(11)
_cell_length_c                   31.0197(11)
_cell_measurement_reflns_used    9785
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.742
_cell_measurement_theta_min      2.849
_cell_volume                     29847.8(18)
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0546
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            228205
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.310
_diffrn_reflns_theta_min         2.014
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.849
_exptl_absorpt_correction_T_max  0.6463
_exptl_absorpt_correction_T_min  0.5572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0964 before and 0.0727 after correction.
The Ratio of minimum to maximum transmission is 0.8621.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.979
_exptl_crystal_description       block
_exptl_crystal_F_000             9144
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 1717 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4595
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1390P)^2^+15.6520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2040
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4097
_reflns_number_total             4595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03345a2.cif
_cod_data_source_block           cx0377
_cod_original_cell_volume        29848(3)
_cod_database_code               7120271
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.751
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O5-C6 \\sim O5A-C6 \\sim O10-C12 \\sim N1-C12 \\sim O10A-C12
 with sigma of 0.02
 O5-C6 \\sim N1A-C6 \\sim O5A-C6 \\sim O10-C12 \\sim N1-C12 \\sim O10A-C12
 with sigma of 0.02
3. Rigid bond restraints
 O5, O5A, O10, O10A, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O5 \\sim O5A \\sim O10 \\sim O10A \\sim N1: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(O5) = Uanis(N1A) = Uanis(O5A) = Uanis(O10) = Uanis(N1) = Uanis(O10A)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(N1)+Sof(H1A)+Sof(H1B)+Sof(H12F)+Sof(H12E)]+1*[Sof(N1A)+Sof(H1AA)+
 Sof(H1AB)+Sof(H6AA)+Sof(H6AB)]=0.25 with esd of 0.0001
 1*[Sof(N1)+Sof(H1A)+Sof(H1B)+Sof(H12F)+Sof(H12E)]+1*[Sof(O10)+Sof(H10)+
 Sof(H12B)+Sof(H12A)]+1*[Sof(O10A)+Sof(H10A)+Sof(H12D)+Sof(H12C)]=1 with esd of
 0.0001
 1*[Sof(N1A)+Sof(H1AA)+Sof(H1AB)+Sof(H6AA)+Sof(H6AB)]+1*[Sof(O5)+Sof(H5)+
 Sof(H6BC)+Sof(H6BD)]+1*[Sof(O5A)+Sof(H5A)+Sof(H6CE)+Sof(H6CF)]=1 with esd of
 0.0001
 Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(H12F)=Sof(H12E)=FVAR(1)
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(H6AA)=Sof(H6AB)=FVAR(2)
 Sof(O10)=Sof(H10)=Sof(H12B)=Sof(H12A)=FVAR(3)
 Sof(O5)=Sof(H5)=Sof(H6BC)=Sof(H6BD)=FVAR(4)
 Sof(O10A)=Sof(H10A)=Sof(H12D)=Sof(H12C)=FVAR(5)
 Sof(O5A)=Sof(H5A)=Sof(H6CE)=Sof(H6CF)=FVAR(6)
 Fixed Sof: Rb1(0.5)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C5(H5B), C7(H7), C8(H8A), C9(H9A),
 C10(H10B), C11(H11)
7.b Secondary CH2 refined with riding coordinates:
 C6(H6BC,H6BD), C6(H6CE,H6CF), C6(H6AA,H6AB), C12(H12B,H12A), C12(H12F,H12E),
 C12(H12D,H12C)
7.c Tetrahedral OH refined with riding coordinates:
 O4(H4), O5(H5), O5A(H5A), O8(H8), O10(H10), O10A(H10A)
7.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N1A(H1AA,H1AB)
7.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O9(H9)
;
_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 = 12922.3 Ang^3^ [43.3%]
Total electron count / cell = 4098.5
;
_shelx_res_checksum              45953
_olex2_date_sample_data_collection 2015-04-01
_olex2_date_sample_submission    2015-04-01
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_original_sample_id KJH_4-146-1-MOF
_olex2_submission_special_instructions 'No special instructions were received'