Exploring porosity in a flexible 3D organic-inorganic {ZnII3(4DPNDI)[W<sup>V</sup>(CN)<sub>8</sub>]<sub>2</sub>} coordination network.
Jędrzejowska, Katarzyna; Kobylarczyk, Jedrzej; Muzioł, Tadeusz M; Nowicka, Beata; Jędrzejowski, Damian; Matoga, Dariusz; Gaweł, Bartłomiej; Podgajny, Robert; Chemical communications (Cambridge, England) 60 (2024) 10704–10707; doi:10.1039/d4cc03141e

data_7133585
_publ_section_title
;
 Exploring porosity in a flexible 3D organic-inorganic
 {ZnII3(4DPNDI)[W<sup>V</sup>(CN)<sub>8</sub>]<sub>2</sub>} coordination
 network.
;
_journal_issue                   77
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10704
_journal_page_last               10707
_journal_paper_doi               10.1039/d4cc03141e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C64 H66 N26 O10 W2 Zn3, 2(C4 H9 N O), [+ solvents]'
_chemical_formula_sum            'C72 H84 N28 O12 W2 Zn3'
_chemical_formula_weight         2097.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-10 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                103.573(2)
_cell_angle_beta                 102.206(2)
_cell_angle_gamma                94.0730(10)
_cell_formula_units_Z            1
_cell_length_a                   9.7937(4)
_cell_length_b                   16.0738(7)
_cell_length_c                   19.6573(9)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.53
_cell_volume                     2916.3(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21253
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.530
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.627
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0888 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.5996.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       block
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.044
_refine_diff_density_min         -2.013
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         10076
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+13.5672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8449
_reflns_number_total             10076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03141e2.cif
_cod_data_source_block           2_DMA
_cod_depositor_comments
'Adding full bibliography for 7133584--7133585.cif.'
_cod_database_code               7133585
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1S-C4S
 1.46 with sigma of 0.02
 C3S-N1S
 1.46 with sigma of 0.02
 H3SB_$1-H3SB
 2 with sigma of 0.02
 C2S-C1S
 1.55 with sigma of 0.02
 H3SC-H2SB
 -2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N7) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(C3S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.03
Uanis(C4S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.03
Uanis(N1S) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(C2S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(O1S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.05
Uanis(C1S) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.2
Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
4.a Aromatic/amide H refined with riding coordinates:
 C5L(H5L), C1L(H1L), C4L(H4L), C2L(H2L), C12L(H12L), C11L(H11L)
4.b Idealised Me refined as rotating group:
 C2CS(H2CA,H2CB,H2CC), C3CS(H3CA,H3CB,H3CC), C4CS(H4CA,H4CB,H4CC), C10C(H10A,
 H10B,H10C), C6CS(H6CA,H6CB,H6CC), C8CS(H8CA,H8CB,H8CC), C12C(H12A,H12B,H12C),
 C11C(H11A,H11B,H11C), C7CS(H7CA,H7CB,H7CC), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,
 H4SC), C3S(H3SA,H3SB,H3SC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27934
_shelx_hkl_checksum              57908
_shelx_fab_checksum              91825
_olex2_submission_special_instructions 'No special instructions were received'