Metal-organic frameworks utilising an interlocked, hexadentate linker containing a tetra-carboxylate axle and a bis(pyridine) wheel.
Gholami, Ghazale; Baggi, Giorgio; Zhu, Kelong; Loeb, Stephen J.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2462–2470; doi:10.1039/c6dt04596k

data_7041967
_publ_section_title
;
 Metal-organic frameworks utilising an interlocked, hexadentate linker
 containing a tetra-carboxylate axle and a bis(pyridine) wheel.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2462
_journal_page_last               2470
_journal_paper_doi               10.1039/c6dt04596k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C48 H30 N4 O10 Zn2, C24 H32 O8, 2(C5 H11 N O), 2(H2 O)'
_chemical_formula_sum            'C82 H88 N6 O22 Zn2'
_chemical_formula_weight         1640.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-01-22 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                97.0926(17)
_cell_angle_beta                 94.778(2)
_cell_angle_gamma                102.6227(18)
_cell_formula_units_Z            1
_cell_length_a                   8.2465(4)
_cell_length_b                   14.4619(6)
_cell_length_c                   16.5490(8)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      31.631
_cell_measurement_theta_min      2.942
_cell_volume                     1898.76(15)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      130.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30083
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.398
_diffrn_reflns_theta_min         2.875
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.7077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0488 before and 0.0397 after correction.
The Ratio of minimum to maximum transmission is 0.9483.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       prism
_exptl_crystal_F_000             858
_exptl_crystal_recrystallization_method 'solvothermal DEF'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7692
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0402P)^2^+3.0172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6374
_reflns_number_total             7692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04596k2.cif
_cod_data_source_block           Zn_6a
_cod_depositor_comments
'Adding full bibliography for 7041965--7041968.cif.'
_cod_database_code               7041967
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O9 \\sim C40 \\sim N3 \\sim C36 \\sim C38 \\sim C40A \\sim C36A \\sim C38A
\\sim C37 \\sim C39 \\sim O9A \\sim C37A \\sim C39A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Same fragment restrains
{O9A, C40A, N3, C36A, C37A, C38A, C39A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O9, C40, N3, C36, C37, C38, C39}
4. Others
 Sof(O9A)=Sof(C40A)=Sof(H40A)=Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=
 Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(O9)=Sof(C40)=Sof(H40)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=
 Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=FVAR(1)
5.a Free rotating group:
 O1W(H1WA,H1WB)
5.b Rotating group:
 O2W(H2WA,H2WB)
5.c Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C49(H49A,H49B), C36(H36A,H36B), C38(H38A,H38B), C36A(H36C,H36D),
 C38A(H38C,H38D)
5.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C12(H12), C13(H13), C15(H15),
 C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C30(H30), C40(H40), C40A(H40A)
5.e Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C37A(H37D,H37E,H37F), C39A(H39D,
 H39E,H39F)
;
_olex2_submission_special_instructions 'No special instructions were received'