Controllable synthesis of isoreticular pillared-layer MOFs based on N-rich triangular prism building units: gas adsorption and luminescent properties
Xie, Wei; Yao, Chan; Shao, Kui-Zhan; Xu, Yan-Hong; Su, Zhong-Min; New Journal of Chemistry 42 (2018) 20056–; doi:10.1039/C8NJ04260H

data_7057922
_publ_section_title
;
 Controllable synthesis of isoreticular pillared-layer MOFs based on
 N-rich triangular prism building units: gas adsorption and luminescent
 properties
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20056
_journal_paper_doi               10.1039/C8NJ04260H
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety
;          
 '0.25(C132 H60 N36 O48 Zn16), 5.5[C3H7NO], 1.5[C2H8N+]'
;
_chemical_formula_sum            'C52.5 H65.5 N16 O17.5 Zn4'
_chemical_formula_weight         1462.19
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-30
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2018.10.25 svn.r3537 for OlexSys, GUI svn.r5585)
;
_audit_update_record
;
2018-11-01 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   20.054(3)
_cell_length_b                   20.054(3)
_cell_length_c                   30.430(5)
_cell_measurement_temperature    292(2)
_cell_volume                     10598(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      292.54
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            88677
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.345
_exptl_absorpt_coefficient_mu    0.942
_exptl_crystal_density_diffrn    0.916
_exptl_crystal_F_000             3010
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         6372
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0398P)^2^+6.1074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5435
_reflns_number_total             6372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04260h2.cif
_cod_data_source_block           22_sq
_cod_depositor_comments          'Adding full bibliography for 7057922.cif.'
_cod_original_cell_volume        10598(4)
_cod_original_formula_sum        'C52.50 H65.50 N16 O17.50 Zn4'
_cod_database_code               7057922
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6849(8)
 0.3151(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
C10A \\sim C10B \\sim C11A \\sim C11B \\sim C9: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(C10B) \\sim Ueq, Uanis(C10A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C11B)=Sof(H11B)=Sof(C10B)=Sof(H10B)=1-FVAR(1)
 Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C4(H4), C10A(H10A), C11A(H11A), C11B(H11B), C10B(H10B)
;
_shelx_res_checksum              39339
_shelx_hkl_checksum              35071
_shelx_fab_checksum              1990
_platon_squeeze_special_details
;
A solvent mask was calculated and 1027 electrons were 
found in a volume of 7830\%A^3 in 1 void. 
This is consistent with the presence of 
5.5[C3H7NO], 1.5[C2H8N+] per formula unit 
which account for 1042 electrons - in reasonable agreement 
with the number of electrons found.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'