Six new metal-organic frameworks with multi-carboxylic acids and imidazole-based spacers: syntheses, structures and properties.
Wang, Feng; Ke, Xiaohuan; Zhao, Jinbo; Deng, Kejian; Leng, Xiaoke; Tian, Zhengfang; Wen, Lili; Li, Dongfeng; Dalton transactions (Cambridge, England : 2003) 40 (2011) 11856–11865; doi:10.1039/c1dt11130b

data_7017351
_publ_section_title
;
 Six new metal-organic frameworks with multi-carboxylic acids and
 imidazole-based spacers: syntheses, structures and properties.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11856
_journal_page_last               11865
_journal_paper_doi               10.1039/c1dt11130b
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C64 H44 N8 O10 Zn2'
_chemical_formula_weight         1215.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.167(4)
_cell_length_b                   26.668(5)
_cell_length_c                   12.453(3)
_cell_measurement_temperature    173(2)
_cell_volume                     6033(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0946
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10509
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.8747
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Colorless
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
In the refinement, the solvent molecules were found
to be seriouly disordered. We have tried to refine
these atoms coordinates many times, but failed each time.
So in the final refinement, the contribution of these unsolved
solvent to the whole structure were treated by using PLATON/SQUEEZE
programm. Further analysis using PLATON indicates that he void
in the unit cell has a volume of 948.1 Ang^3
(consisting of about 15.7% of the crystal volume,
equally distributed across two cavities).
The residual electron density count amounted to 462 e per unit cell,
corresponding to nearly 8 molecules of DMF and 14 molecules of H2O
(the content of each of the two cavities per unit cell being equivalent
about 4 molecules of DMF and 7 molecules of H2O, i.e. every molecule
is distributed with 2 molecules of DMF and 3.5 molecules of H2O).

W: Number of unusual anisotropic displacement parameters ................. 2
N: Total Potential Solvent Accessible Void Vol .................. 948.1 Ang^3
N: Electron Count / Cell = 461 - To be included in D(calc), F000 & Mol.Wght.
;
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.038(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         10509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+5.3679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                8771
_reflns_number_total             10509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11130b.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2
_cod_database_code               7017351