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_7041968
_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 H28 N4 O8, 2(H2 O), C34 H38 N2 O8, 1.5(C5 H11 N O), Cu'
_chemical_formula_sum            'C89.5 H86.5 Cu N7.5 O19.5'
_chemical_formula_weight         1641.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-25 deposited with the CCDC.
2017-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.263(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.2427(6)
_cell_length_b                   14.0544(5)
_cell_length_c                   17.5540(6)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      78.12
_cell_measurement_theta_min      2.63
_cell_volume                     4140.5(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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.35
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.898
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28562
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        65.075
_diffrn_reflns_theta_max         65.075
_diffrn_reflns_theta_min         3.240
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.6255
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1170 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.8294.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       prism
_exptl_crystal_F_000             1727
_exptl_crystal_recrystallization_method 'solvothermal from DEF, EtOH, H2O'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.493
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     2324
_refine_ls_restrained_S_all      1.314
_refine_ls_R_factor_all          0.1677
_refine_ls_R_factor_gt           0.1245
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3433
_refine_ls_wR_factor_ref         0.3856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3945
_reflns_number_total             6343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04596k2.cif
_cod_data_source_block           cu_gg004_0m
_cod_depositor_comments
'Adding full bibliography for 7041965--7041968.cif.'
_cod_database_code               7041968
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H64A of C64A, H52C of C52B, H56B of C56B, H66A of C66A,
  H67A of C67A, H68A of C68A, H59B of C59B, H66B of C66B, H56A of C56A, H53D of
  C53B, H54B of C54B, H64B of C64B, H68B of C68B, H59A of C59A, H58A of C58A,
  H58B of C58B, H67B of C67B, H54A of C54A, H53B of C53A, H73 of C73, H72 of
  C72, H54 of C54, H52B of C52A, H53A of C53, H52 of C52, H64 of C64, H67 of
  C67, H59 of C59, H66 of C66, H68 of C68, H56 of C56, H58 of C58, H22A of C22A,
   H21 of C21, H24A of C24A, H23A of C23A, H23 of C23, H1E of C1E, H22 of C22,
  H21A of C21A, H24 of C24, H1D of C1D, H5 of C5, H3 of C3, H7 of C7, All N(H,H,
  H) groups, All Cu(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H0AA of C69B, All O(H) groups
2. Restrained distances
 N1D-C1D
 1.36 with sigma of 0.02
 C1D-O1D
 1.22 with sigma of 0.02
 N1E-C1E
 1.36 with sigma of 0.02
 C1E-O1E
 1.22 with sigma of 0.02
 N1D-C2D \\sim N1D-C4D
 with sigma of 0.02
 C2D-C3D \\sim C4D-C5D
 with sigma of 0.02
 N1E-C2E \\sim N1E-C4E
 with sigma of 0.02
 C2E-C3E \\sim C4E-C5E
 with sigma of 0.02
3. Restrained planarity
 N20, C20, C21, C22, C23, C24
 with sigma of 0.1
 N50, N51, C70, C57, C58, C59, C60, C61, C62
 with sigma of 0.1
 O50, O51, C50, C51
 with sigma of 0.1
 C50, C51, C52, C53, C54, C55, C56
 with sigma of 0.1
 O50A, O51A, C50A, C51A
 with sigma of 0.1
 C50A, C51A, C52A, C53A, C54A, C55A, C56A
 with sigma of 0.1
 O50B, O51B, C50B, C51B
 with sigma of 0.1
 C50B, C51B, C52B, C53B, C54B, C55B, C56B
 with sigma of 0.1
 C57A, C58A, C59A, C60A, C61A, C62A
 with sigma of 0.1
 C57B, C58B, C59B, C60B, C61B, C62B
 with sigma of 0.1
 O52, O53, C65, C69
 with sigma of 0.1
 O52A, O53A, C65A, C69A
 with sigma of 0.1
 O52B, O53B, C65B, C69B
 with sigma of 0.1
 C63A, C64A, C65A, C66A, C67A, C68A, C69A
 with sigma of 0.1
 C63B, C64B, C65B, C66B, C67B, C68B, C69B
 with sigma of 0.1
 C63, C64, C65, C66, C67, C68, C69
 with sigma of 0.1
 O1D, N1D, C1D, C2D, C4D
 with sigma of 0.1
 O1E, N1E, C1E, C2E, C4E
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N20 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim N20A \\sim C20A
\\sim C21A \\sim C22A \\sim C23A \\sim C24A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O50 \\sim O51 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim
C56 \\sim O50A \\sim O51A \\sim C50A \\sim C51A \\sim C52A \\sim C53A \\sim
C54A \\sim C55A \\sim C56A \\sim O50B \\sim O51B \\sim C50B \\sim C51B \\sim
C52B \\sim C53B \\sim C54B \\sim C55B \\sim C56B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
O52 \\sim O53 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim
C69 \\sim O52A \\sim O53A \\sim C63A \\sim C64A \\sim C65A \\sim C66A \\sim
C67A \\sim C68A \\sim C69A \\sim O52B \\sim O53B \\sim C63B \\sim C64B \\sim
C65B \\sim C66B \\sim C67B \\sim C68B \\sim C69B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C57A \\sim C58A
\\sim C59A \\sim C60A \\sim C61A \\sim C62A \\sim C57B \\sim C58B \\sim C59B
\\sim C60B \\sim C61B \\sim C62B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O1D \\sim N1D \\sim C1D \\sim C2D \\sim C3D \\sim C4D \\sim C5D: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O1E \\sim N1E \\sim C1E \\sim C2E \\sim C3E \\sim C4E \\sim C5E: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O51A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O52A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O53A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O52B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O53B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C3E) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C4E) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C50B) = Uanis(O51A) = Uanis(O51)
Uanis(C55A) = Uanis(C55) = Uanis(C55B)
Uanis(C54A) = Uanis(C54B) = Uanis(C54)
Uanis(C50) = Uanis(C50A)
5. Rigid body (RIGU) restrains
 O1D, N1D, C1D, C2D, C3D, C4D, C5D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1E, N1E, C1E, C2E, C3E, C4E, C5E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{N50, N51, C70, O50A, O51A, O52A, O53A, C50A, C51A, C52A, C53A, C54A, C55A,
C56A, C57A, C58A, C59A, C60A, C61A, C62A, C63A, C64A, C65A, C66A, C67A, C68A,
C69A} sigma for 1-2: 0.02, 1-3: 0.02
{N50, N51, C70, O50B, O51B, O52B, O53B, C50B, C51B, C52B, C53B, C54B, C55B,
C56B, C57B, C58B, C59B, C60B, C61B, C62B, C63B, C64B, C65B, C66B, C67B, C68B,
C69B} sigma for 1-2: 0.02, 1-3: 0.02
as
{N50, N51, C70, O50, O51, O52, O53, C50, C51, C52, C53, C54, C55, C56, C57,
C58, C59, C60, C61, C62, C63, C64, C65, C66, C67, C68, C69}
{N20A, C20A, C21A, C22A, C23A, C24A} sigma for 1-2: 0.02, 1-3: 0.02
as
{N20, C20, C21, C22, C23, C24}
{O1E, N1E, C1E, C2E, C3E, C4E, C5E} sigma for 1-2: 0.02, 1-3: 0.02
as
{O1D, N1D, C1D, C2D, C3D, C4D, C5D}
7. Others
 1*[Sof(H51)+Sof(O50)+Sof(O51)+Sof(O52)+Sof(O53)+Sof(H53)+Sof(C50)+Sof(C51)+
 Sof(C52)+Sof(H52)+Sof(C53)+Sof(H53A)+Sof(C54)+Sof(H54)+Sof(C55)+Sof(C56)+
 Sof(H56)+Sof(C57)+Sof(C58)+Sof(H58)+Sof(C59)+Sof(H59)+Sof(C60)+Sof(C61)+
 Sof(C62)+Sof(C63)+Sof(C64)+Sof(H64)+Sof(C65)+Sof(C66)+Sof(H66)+Sof(C67)+
 Sof(H67)+Sof(C68)+Sof(H68)+Sof(C69)+Sof(O1E)+Sof(N1E)+Sof(C1E)+Sof(H1E)+
 Sof(C2E)+Sof(H2EA)+Sof(H2EB)+Sof(C3E)+Sof(H3EA)+Sof(H3EB)+Sof(H3EC)+Sof(C4E)+
 Sof(H4EA)+Sof(H4EB)+Sof(C5E)+Sof(H5EA)+Sof(H5EB)+Sof(H5EC)]+1*[Sof(H51A)+
 Sof(O50A)+Sof(O51A)+Sof(O52A)+Sof(H52A)+Sof(O53A)+Sof(C50A)+Sof(C51A)+
 Sof(C52A)+Sof(H52B)+Sof(C53A)+Sof(H53B)+Sof(C54A)+Sof(H54A)+Sof(C55A)+
 Sof(C56A)+Sof(H56A)+Sof(C57A)+Sof(C58A)+Sof(H58A)+Sof(C59A)+Sof(H59A)+
 Sof(C60A)+Sof(C61A)+Sof(C62A)+Sof(C63A)+Sof(C64A)+Sof(H64A)+Sof(C65A)+
 Sof(C66A)+Sof(H66A)+Sof(C67A)+Sof(H67A)+Sof(C68A)+Sof(H68A)+Sof(C69A)]+1*
 [Sof(H51B)+Sof(O50B)+Sof(O51B)+Sof(O52B)+Sof(O53B)+Sof(H53C)+Sof(C50B)+
 Sof(C51B)+Sof(C52B)+Sof(H52C)+Sof(C53B)+Sof(H53D)+Sof(C54B)+Sof(H54B)+
 Sof(C55B)+Sof(C56B)+Sof(H56B)+Sof(C57B)+Sof(C58B)+Sof(H58B)+Sof(C59B)+
 Sof(H59B)+Sof(C60B)+Sof(C61B)+Sof(C62B)+Sof(C63B)+Sof(C64B)+Sof(H64B)+
 Sof(C65B)+Sof(C66B)+Sof(H66B)+Sof(C67B)+Sof(H67B)+Sof(C68B)+Sof(H68B)+
 Sof(C69B)+Sof(O1D)+Sof(N1D)+Sof(C1D)+Sof(H1D)+Sof(C2D)+Sof(H2DA)+Sof(H2DB)+
 Sof(C3D)+Sof(H3DA)+Sof(H3DB)+Sof(H3DC)+Sof(C4D)+Sof(H4DA)+Sof(H4DB)+Sof(C5D)+
 Sof(H5DA)+Sof(H5DB)+Sof(H5DC)]=1 with esd of 0.0001
 Sof(N20A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=
 Sof(H23A)=Sof(C24A)=Sof(H24A)=1-FVAR(1)
 Sof(N20)=Sof(C20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=
 Sof(C24)=Sof(H24)=FVAR(1)
 Sof(H51)=Sof(O50)=Sof(O51)=Sof(O52)=Sof(O53)=Sof(H53)=Sof(C50)=Sof(C51)=
 Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53A)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(C56)=
 Sof(H56)=Sof(C57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(C61)=
 Sof(C62)=Sof(C63)=Sof(C64)=Sof(H64)=Sof(C65)=Sof(C66)=Sof(H66)=Sof(C67)=
 Sof(H67)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(O1E)=Sof(N1E)=Sof(C1E)=Sof(H1E)=
 Sof(C2E)=Sof(H2EA)=Sof(H2EB)=Sof(C3E)=Sof(H3EA)=Sof(H3EB)=Sof(H3EC)=Sof(C4E)=
 Sof(H4EA)=Sof(H4EB)=Sof(C5E)=Sof(H5EA)=Sof(H5EB)=Sof(H5EC)=FVAR(2)
 Sof(H51A)=Sof(O50A)=Sof(O51A)=Sof(O52A)=Sof(H52A)=Sof(O53A)=Sof(C50A)=
 Sof(C51A)=Sof(C52A)=Sof(H52B)=Sof(C53A)=Sof(H53B)=Sof(C54A)=Sof(H54A)=
 Sof(C55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=
 Sof(H59A)=Sof(C60A)=Sof(C61A)=Sof(C62A)=Sof(C63A)=Sof(C64A)=Sof(H64A)=
 Sof(C65A)=Sof(C66A)=Sof(H66A)=Sof(C67A)=Sof(H67A)=Sof(C68A)=Sof(H68A)=
 Sof(C69A)=FVAR(3)
 Sof(H51B)=Sof(O50B)=Sof(O51B)=Sof(O52B)=Sof(O53B)=Sof(H53C)=Sof(C50B)=
 Sof(C51B)=Sof(C52B)=Sof(H52C)=Sof(C53B)=Sof(H53D)=Sof(C54B)=Sof(H54B)=
 Sof(C55B)=Sof(C56B)=Sof(H56B)=Sof(C57B)=Sof(C58B)=Sof(H58B)=Sof(C59B)=
 Sof(H59B)=Sof(C60B)=Sof(C61B)=Sof(C62B)=Sof(C63B)=Sof(C64B)=Sof(H64B)=
 Sof(C65B)=Sof(C66B)=Sof(H66B)=Sof(C67B)=Sof(H67B)=Sof(C68B)=Sof(H68B)=
 Sof(C69B)=Sof(O1D)=Sof(N1D)=Sof(C1D)=Sof(H1D)=Sof(C2D)=Sof(H2DA)=Sof(H2DB)=
 Sof(C3D)=Sof(H3DA)=Sof(H3DB)=Sof(H3DC)=Sof(C4D)=Sof(H4DA)=Sof(H4DB)=Sof(C5D)=
 Sof(H5DA)=Sof(H5DB)=Sof(H5DC)=FVAR(4)
 Fixed Sof: Cu1(0.5)
 Fixed X: H0AA(0.05464) H0AB(0.07598)
 Fixed Y: H0AA(0.50368) H0AB(0.53537)
 Fixed Z: H0AA(-0.273) H0AB(-0.195411)
8.a Riding coordinates:
 O53(H53), O52A(H52A), C3E(H3EA,H3EB,H3EC), C5E(H5EA,H5EB,H5EC), C3D(H3DA,H3DB,
 H3DC)
8.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C2E(H2EA,H2EB), C4E(H4EA,H4EB), C2D(H2DA,H2DB), C4D(H4DA,H4DB)
8.c Aromatic/amide H refined with riding coordinates:
 N51(H51), N51(H51A), N51(H51B), C52(H52), C53(H53A), C54(H54), C56(H56),
 C58(H58), C59(H59), C64(H64), C66(H66), C67(H67), C68(H68), C72(H72), C73(H73),
  C52A(H52B), C53A(H53B), C54A(H54A), C56A(H56A), C58A(H58A), C59A(H59A),
 C64A(H64A), C66A(H66A), C67A(H67A), C68A(H68A), C52B(H52C), C53B(H53D),
 C54B(H54B), C56B(H56B), C58B(H58B), C59B(H59B), C64B(H64B), C66B(H66B),
 C67B(H67B), C68B(H68B), C3(H3), C5(H5), C7(H7), C21(H21), C22(H22), C23(H23),
 C24(H24), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C1E(H1E), C1D(H1D)
8.d Idealised Me refined as rotating group:
 C5D(H5DA,H5DB,H5DC)
8.e Idealised tetrahedral OH refined as rotating group:
 O53B(H53C)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'