Solvent-induced single-crystal to single-crystal transformation of a Zn4O-containing doubly interpenetrated metal‒organic framework with a pcu net
Lee, Jae Hwa; Kim, Tae Kyung; Suh, Myunghyun Paik; Moon, Hoi Ri; CrystEngComm 17 (2015) 8807–; doi:10.1039/C5CE01074H

data_7221688
_publ_section_title
;
 Solvent-induced single-crystal to single-crystal transformation of a
 Zn4O-containing doubly interpenetrated metal--organic framework with a
 pcu net
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8807
_journal_paper_doi               10.1039/C5CE01074H
_journal_volume                  17
_journal_year                    2015
_chemical_compound_source
'Zinc nitrate hexahydrate, bis(4-carboxyphenyl)-N-methylamine'
_chemical_formula_moiety         'C90 H66 N6 O26 Zn8, 8 (C3 H7 N O)'
_chemical_formula_sum            'C114 H122 N14 O34 Zn8'
_chemical_formula_weight         2755.22
_chemical_name_common            Zn4OCPMA_origin
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-25 deposited with the CCDC.
2015-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.985(3)
_cell_length_b                   18.985(3)
_cell_length_c                   68.340(14)
_cell_measurement_reflns_used    125758
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.385
_cell_measurement_theta_min      1.908
_cell_volume                     21332(6)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'MS Modeling'
_computing_publication_material  WinGX
_computing_structure_refinement  'Bruker SHELXTL-XL'
_computing_structure_solution    'Bruker SHELXTL-XS'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       94
_diffrn_reflns_limit_l_min       -94
_diffrn_reflns_number            65641
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.339
_exptl_absorpt_correction_T_max  0.7755
_exptl_absorpt_correction_T_min  0.7055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Length, width, and breadth roughly equal'
_exptl_crystal_F_000             8496
_exptl_crystal_recrystallization_method 'Solvothermal synthesis'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
 The contribution of some 1870 electrons were removed by the SQUEEZE process. In space group R32, this then implies that the some 1870/18 = 103.9 of the removed electrons would be associated with the asymmetric unit and hence that 103.9/40 = 2.6 molecules of N,N-dimethylformamide (DMF) would be associated with the asymmetric unit. As the value of Z is 6 and a Zn~8~ formula unit has 3 asymmetric units, this would then imply that the contribution of some 8 molecules of DMF were removed from the formula unit by the SQUEEZE process. Therefore, the formulation appear as [Zn~4~O(CPMA)~3~]~2~ 8DMF.
;
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.061(15)
_refine_ls_extinction_coef       0.00110(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         12870
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1835
_reflns_number_gt                7991
_reflns_number_total             12870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01074h2.cif
_cod_data_source_block           zn4ocpma_origin_r32_sqd
_cod_depositor_comments
'Adding full bibliography for 7221688--7221691.cif.'
_cod_original_cell_volume        21331(6)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               7221688
_platon_squeeze_void_probe_radius 1.20