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_7221690
_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         'C45 H33 N3 O13 Zn4, 3(C3 H7), 3(C3 H7)'
_chemical_formula_sum            'C63 H75 N3 O13 Zn4'
_chemical_formula_weight         1343.74
_chemical_name_common            Zn4OCPMA_hexane
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :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            12
_cell_length_a                   18.653(3)
_cell_length_b                   18.653(3)
_cell_length_c                   65.066(13)
_cell_measurement_reflns_used    157199
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.803
_cell_measurement_theta_min      2.274
_cell_volume                     19606(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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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     0.67999
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       94
_diffrn_reflns_limit_l_min       -94
_diffrn_reflns_number            77769
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.7848
_exptl_absorpt_correction_T_min  0.7220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Length, width, and breadth roughly equal'
_exptl_crystal_F_000             8376
_exptl_crystal_recrystallization_method 'Solvothermal synthesis'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.345
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.00350(17)
_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   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         8067
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0575
_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^)+(0.1335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1753
_reflns_number_gt                5700
_reflns_number_total             8067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01074h2.cif
_cod_data_source_block           zn4ocpma_hx_r-3c
_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_cell_volume        19605(6)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7221690