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_7041965
_publ_section_title
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 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 O8, C24 H32 O8, 1.6(C3 H7 N O)'
_chemical_formula_sum            'C76.8 H73.2 N5.6 O17.6'
_chemical_formula_weight         1356.21
_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   geom
_atom_sites_solution_primary     dual
_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                76.9517(16)
_cell_angle_beta                 79.6241(15)
_cell_angle_gamma                81.520(2)
_cell_formula_units_Z            1
_cell_length_a                   8.0014(3)
_cell_length_b                   14.3032(6)
_cell_length_c                   15.5636(8)
_cell_measurement_reflns_used    4408
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.94
_cell_volume                     1696.19(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.2
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.914
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10864
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.346
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7011
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       rectanglar
_exptl_crystal_F_000             714
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.6939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4784
_reflns_number_total             6336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04596k2.cif
_cod_data_source_block           6a_DMF
_cod_depositor_comments
'Adding full bibliography for 7041965--7041968.cif.'
_cod_original_formula_sum        'C76.80 H73.20 N5.60 O17.60'
_cod_database_code               7041965
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.978
_exptl_absorpt_special_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0425 before and 0.0364 after correction.
The Ratio of minimum to maximum transmission is 0.9403.
The \l/2 correction factor is 0.00150.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(H04I)=Sof(H04J)=Sof(C0)=Sof(H0A)=Sof(H0B)=1-FVAR(1)
 Sof(H04G)=Sof(H04H)=Sof(C049)=Sof(H04K)=Sof(H04L)=FVAR(1)
 Fixed Sof: O047(0.8) N044(0.8) C048(0.8) H048(0.8) C050(0.8) H05A(0.8)
 H05B(0.8) H05C(0.8) C051(0.8) H05D(0.8) H05E(0.8) H05F(0.8)
3.a Secondary CH2 refined with riding coordinates:
 C038(H03A,H03B), C042(H04A,H04B), C043(H04C,H04D), C045(H04E,H04F), C046(H04G,
 H04H), C046(H04I,H04J), C049(H04K,H04L), C0(H0A,H0B)
3.b Aromatic/amide H refined with riding coordinates:
 N006(H006), C014(H014), C015(H015), C016(H016), C022(H022), C025(H025),
 C026(H026), C028(H028), C029(H029), C031(H031), C033(H033), C034(H034),
 C037(H037), C035(H035), C036(H036), C039(H039), C041(H041), C048(H048)
3.c Idealised Me refined as rotating group:
 C050(H05A,H05B,H05C), C051(H05D,H05E,H05F)
3.d Idealised tetrahedral OH refined as rotating group:
 O004(H004), O005(H005)
;
_olex2_submission_special_instructions 'No special instructions were received'