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_7221689
_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         '2 (C90 H66 N6 O26 Zn8), 31 (C6 H6)'
_chemical_formula_sum            'C366 H318 N12 O52 Zn16'
_chemical_formula_weight         6762.24
_chemical_name_common            Zn4OCPMA_benzene
_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            3
_cell_length_a                   19.168(3)
_cell_length_b                   19.168(3)
_cell_length_c                   67.695(13)
_cell_measurement_reflns_used    99958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.601
_cell_measurement_theta_min      1.244
_cell_volume                     21540(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.70001
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            48637
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.8246
_exptl_absorpt_correction_T_min  0.7575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Length, width, and breadth roughly equal'
_exptl_crystal_F_000             10482
_exptl_crystal_recrystallization_method 'Solvothermal synthesis'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
 The contribution of some 3520 electrons were removed by the SQUEEZE process. In space group R32, this then implies that the some 3520/18 = 195.6 of the removed electrons would be associated with the asymmetric unit and hence that 195.6/42 = 4.66 molecules of benzene would be associated with the asymmetric unit. As the value of Z is 3 and a Zn~16~ formula unit has 6 asymmetric units, this would then imply that the contribution of some 28 molecules of DMF were removed from the formula unit by the SQUEEZE process. It is also noted that the present asymmetric unit does contain the contributions of Zn~2.67~ and half of a benzene molecule. Thus a Zn~16~ formulation would have an additional 3 benzene molecules already present. Therefore, the formulation appear as [Zn~4~O(CPMA)~3~]~4~ 31benezene.
;
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(2)
_refine_ls_extinction_coef       0.00028(6)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         8835
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1194P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                6125
_reflns_number_total             8835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01074h2.cif
_cod_data_source_block           zn4ocpma_bz_r32_sqd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7221688--7221691.cif.
;
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               7221689
_platon_squeeze_void_probe_radius 1.20