A New Multidentate Hexacarboxylic Acid for the Construction of Porous Metal−Organic Frameworks of Diverse Structures and Porosities
Chen, Zhenxia; Xiang, Shengchang; Liao, Tengbiao; Yang, Yongtai; Chen, Yu-Sheng; Zhou, Yaming; Zhao, Dongyuan; Chen, Banglin; Crystal Growth & Design 10 (2010) 2775–; doi:10.1021/cg100316s

data_4501714
_publ_section_title
;
 A New Multidentate Hexacarboxylic Acid for the Construction of Porous
 Metal&#x2212;Organic Frameworks of Diverse Structures and Porosities
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2775
_journal_paper_doi               10.1021/cg100316s
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C40.50 H39 N3 O16.50 Zn3'
_chemical_formula_sum            'C40.5 H39 N3 O16.5 Zn3'
_chemical_formula_weight         1027.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           161
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   22.602(3)
_cell_length_b                   22.602(3)
_cell_length_c                   39.721(8)
_cell_measurement_reflns_used    587
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      24.129
_cell_measurement_theta_min      2.236
_cell_volume                     17573(5)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_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      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0383
_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       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            49068
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             6300
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
Although there were five peaks within the void from Fourier difference map,
the highly disordered solvents within the void were not crystallographically
well defined.

The SQUEEZE routine of the program PLATON was used
in order to eliminate the contribution of disordered solvents molecules,
thereby a final model based only on the ordered part of the crystal structure
was obtained.

The SQUEEZE routine suggested that
a total potential solvent area volume of 7182.0 Ang^3^[40.9% of cell volume],
and a void electron population of 108 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.1118 for >2sigma(I) data
R1 = 0.1168, wR2 = 0.3195, GooF = S = 1.397 for all data
( 8918 data and 1 restraint / 330 parameters)
;
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8542
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0797P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                7587
_reflns_number_total             8542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100316s_si_002.cif
_cod_data_source_block           MOF2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      R3c
_cod_original_formula_sum        'C40.50 H39 N3 O16.50 Zn3'
_cod_database_code               4501714