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_7041966
_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         '0.5(C164 H128 N12 O32 Zn4), 2(C5 H11 N O)'
_chemical_formula_sum            'C102 H108 N10 O20 Zn2'
_chemical_formula_weight         1924.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 95.4192(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4221(4)
_cell_length_b                   21.2742(8)
_cell_length_c                   19.0647(7)
_cell_measurement_reflns_used    9299
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.981
_cell_measurement_theta_min      3.120
_cell_volume                     4611.9(3)
_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      173.0
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24228
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        60.073
_diffrn_reflns_theta_max         60.073
_diffrn_reflns_theta_min         3.120
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.5818
_exptl_absorpt_correction_T_min  0.4908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1365 before and 0.1141 after correction.
The Ratio of minimum to maximum transmission is 0.8436.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       prism
_exptl_crystal_F_000             2020
_exptl_crystal_recrystallization_method 'solvothermal DEF'
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         6673
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1120P)^2^+4.6528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5024
_reflns_number_total             6673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04596k2.cif
_cod_data_source_block           Zn_6c
_cod_depositor_comments
'Adding full bibliography for 7041965--7041968.cif.'
_cod_database_code               7041966
_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
2. Restrained distances
 C2S-C1S
 1.4 with sigma of 0.005
3. Restrained planarity
 N1S, C0AA, C1S, C3SA
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1S \\sim N1S \\sim C0AA \\sim C1S \\sim C2S \\sim C3SA \\sim C4SA \\sim C3SB
\\sim C4SB: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Same fragment restrains
{N1S, C0AA, C3SA, C4SA} sigma for 1-2: 0.02, 1-3: 0.02
{N1S, C0AA, C3SB, C4SB} sigma for 1-2: 0.02, 1-3: 0.02
as
{N1S, C0AA, C1S, C2S}
6. Others
 Sof(C3SB)=Sof(H3SC)=Sof(H3SD)=Sof(C4SB)=Sof(H4SD)=Sof(H4SE)=Sof(H4SF)=1-FVAR(1)
 Sof(C3SA)=Sof(H3SA)=Sof(H3SB)=Sof(C4SA)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=FVAR(1)
7.a Riding coordinates:
 C4SA(H4SA,H4SB,H4SC)
7.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C1S(H1SA,H1SB), C3SA(H3SA,H3SB), C3SB(H3SC,H3SD)
7.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C19(H19), C23(H23), C24(H24), C26(H26), C28(H28), C30(H30),
  C38(H38), C39(H39), C40(H40), C41(H41), C0AA(H0AA)
7.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C4SB(H4SD,H4SE,H4SF)
;
_olex2_submission_special_instructions 'No special instructions were received'