A porous framework based on tetrakis(4-pyridyloxymethyl)methane fine-tuned by metal ions: synthesis, crystal structures and adsorption properties
Li, Zhao; Chen, Xi; Yu, Fan; Su, Min; Zhang, Bi-quan; Li, Bao; Zhang, Tian-le; New J. Chem. 40 (2016) 1430–; doi:10.1039/C5NJ02002F

data_7055181
_publ_section_title
;
 A porous framework based on tetrakis(4-pyridyloxymethyl)methane
 fine-tuned by metal ions: synthesis, crystal structures and adsorption
 properties
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1430
_journal_paper_doi               10.1039/C5NJ02002F
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C53 H48 Cd2 N4 O16,8(H2O)'
_chemical_formula_sum            'C53 H64 Cd2 N14 O24'
_chemical_formula_weight         1505.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-17 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.48
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   46.403
_cell_length_b                   11.125
_cell_length_c                   24.144
_cell_measurement_reflns_used    7075
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.715
_cell_measurement_theta_min      2.877
_cell_volume                     12327.675
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker APEX-II CCD'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.1214
_diffrn_reflns_av_unetI/netI     0.1378
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44145
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.874
_exptl_absorpt_coefficient_mu    0.761
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             5104
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         12130
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1021P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.2178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5633
_reflns_number_total             12130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02002f2.cif
_cod_data_source_block           COMPOUND3
_cod_depositor_comments
'Adding full bibliography for 7055179--7055181.cif.'
_cod_original_cell_volume        12327.7
_cod_database_code               7055181
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O12A-C47A = O13A-C47A = C47A-C48A
 1.4 with sigma of 0.01
 O12B-C47B = O13B-C47B = C47B-C48B
 1.4 with sigma of 0.01
 O12B-C48B = O13B-C48B = C47B-C49B = C47B-C53B
 2.45 with sigma of 0.02
 C51B-O14B
 1.4 with sigma of 0.01
 O14B-C50B = O14B-C52B
 2.4 with sigma of 0.02
 C48B-C49B = C49B-C50B = C50B-C51B = C51B-C52B = C52B-C53B
 1.4 with sigma of 0.02
 C48B-C50B = C49B-C51B = C50B-C52B = C51B-C53B = C52B-C48B = C53B-C49B
 2.4 with sigma of 0.02
 C51A-O14A
 1.4 with sigma of 0.01
 O14A-C50A = O14A-C52A
 2.4 with sigma of 0.02
 O14B-C43B
 2.4 with sigma of 0.02
 C44B-O14B
 1.4 with sigma of 0.01
 O12A-C48A = O13A-C48A = C47A-C49A = C47A-C53A
 2.45 with sigma of 0.02
 C48A-C49A = C49A-C50A = C50A-C51A = C51A-C52A = C52A-C53A
 1.4 with sigma of 0.02
 C48A-C50A = C49A-C51A = C50A-C52A = C51A-C53A = C52A-C48A = C53A-C49A
 2.4 with sigma of 0.02
3. Restrained planarity
 C47A, C48A, O13A, O12A
 with sigma of 0.1
 C47B, C48B, O13B, O12B
 with sigma of 0.1
 C47B, C48B, C49B, C53B
 with sigma of 0.1
 C48B, C49B, C50B, C51B, C52B, C53B
 with sigma of 0.1
 C50B, C51B, C52B, O14B
 with sigma of 0.1
 C50A, C51A, C52A, O14A
 with sigma of 0.1
 C46, C41, C42, O14A
 with sigma of 0.1
 C46, C41, C42, C43B, C44B, O14B
 with sigma of 0.1
 C47A, C48A, C49A, C53A
 with sigma of 0.1
 C48A, C49A, C50A, C51A, C52A, C53A
 with sigma of 0.1
4. Rigid bond restraints
 C47A, O13A, O12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C47B, C48B, C49B, C50B, C51B, C52B, C53B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C47B, O13B, O12B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C50B, C51B, C52B, O14B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C50A, C51A, C52A, O14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C46, C41, C42, O14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C46, C41, C42, C43B, C44B, O14B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C47A, C48A, C49A, C50A, C51A, C52A, C53A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C47A \\sim O13A \\sim O12A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C47B \\sim C48B \\sim C49B \\sim C50B \\sim C51B \\sim C52B \\sim C53B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C47B \\sim O13B \\sim O12B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C50B \\sim C51B \\sim C52B \\sim O14B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C50A \\sim C51A \\sim C52A \\sim O14A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C46 \\sim C41 \\sim C42 \\sim O14A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C46 \\sim C41 \\sim C42 \\sim C43B \\sim C44B \\sim O14B: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C47A \\sim C48A \\sim C49A \\sim C50A \\sim C51A \\sim C52A \\sim C53A: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C45A) \\sim Ueq, Uanis(C45B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Others
 Sof(C43B)=Sof(H43B)=Sof(C44B)=Sof(C45B)=Sof(H45B)=Sof(C47B)=Sof(C48B)=
 Sof(C49B)=Sof(H49B)=Sof(C50B)=Sof(H50B)=Sof(C51B)=Sof(C52B)=Sof(H52B)=
 Sof(C53B)=Sof(H53B)=Sof(O14B)=Sof(O13B)=Sof(O12B)=1-FVAR(1)
 Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(C45A)=Sof(H45A)=Sof(C47A)=Sof(C48A)=
 Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(C52A)=Sof(H52A)=
 Sof(C53A)=Sof(H53A)=Sof(O14A)=Sof(O13A)=Sof(O12A)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C18(H18A,H18B), C12(H12A,H12B), C24(H24A,H24B)
7.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C32(H32), C38(H38), C35(H35), C19(H19), C39(H39), C22(H22),
 C29(H29), C20(H20), C16(H16), C31(H31), C36(H36), C10(H10), C5(H5), C17(H17),
 C28(H28), C23(H23), C11(H11), C13(H13), C2(H2), C4(H4), C8(H8), C1(H1), C7(H7),
  C43A(H43A), C45A(H45A), C49A(H49A), C50A(H50A), C52A(H52A), C53A(H53A),
 C43B(H43B), C45B(H45B), C49B(H49B), C50B(H50B), C52B(H52B), C53B(H53B)
;
_shelx_fab_checksum              22161
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'