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_4501715
_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         'C33 H26 Cd3 N O17'
_chemical_formula_sum            'C33 H26 Cd3 N O17'
_chemical_formula_weight         1045.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 112.301(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.476(11)
_cell_length_b                   23.135(8)
_cell_length_c                   18.163(6)
_cell_measurement_reflns_used    2417
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      18.36
_cell_measurement_theta_min      2.69
_cell_volume                     12626(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1478
_diffrn_reflns_av_sigmaI/netI    0.1562
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16448
_diffrn_reflns_theta_full        19.64
_diffrn_reflns_theta_max         19.64
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  0.9026
_exptl_absorpt_correction_T_min  0.8181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Although there were seven 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 6985.8 Ang^3^[55.3% of cell volume],
and a void electron population of 2972 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.1216 for >2sigma(I) data
R1 = 0.1818, wR2 = 0.3656, GooF = S = 1.250 for all data
( 5582 data and 0 restraint / 554 parameters)
;
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5582
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0683P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                3238
_reflns_number_total             5582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100316s_si_003.cif
_cod_data_source_block           MOF3
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4501715