Two unprecedented porous anionic frameworks: organoammonium templating effects and structural diversification
Hao, Xiang-Rong; Wang, Xin-Long; Su, Zhong-Min; Shao, Kui-Zhan; Zhao, Ya-Hui; Lan, Ya-Qian; Fu, Yao-Mei; Dalton Transactions  (2009) 8562–8566; doi:10.1039/b906728k

data_7002482
_publ_section_title
;
 Two unprecedented porous anionic frameworks: organoammonium templating
 effects and structural diversification
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8562
_journal_page_last               8566
_journal_paper_doi               10.1039/b906728k
_journal_year                    2009
_chemical_formula_moiety         '(C24 Cd2 N3 O12), 4(C2 H8 N), 8(C4 H9 N O)'
_chemical_formula_sum            'C44 H64 Cd2 N9 O16'
_chemical_formula_weight         1199.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           65
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2'
_symmetry_space_group_name_H-M   'C m m m'
_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            2
_cell_length_a                   16.835(4)
_cell_length_b                   14.862(4)
_cell_length_c                   14.532(4)
_cell_measurement_reflns_used    3588
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      3.56
_cell_volume                     3635.9(16)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Smart Apex2 CCD'
_diffrn_measurement_method       'phi and omega 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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10749
_diffrn_reflns_theta_full        27.33
_diffrn_reflns_theta_max         27.33
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as guest

atoms were unsuccessful. The data were corrected for disordered

electron density through use of the SQUEEZE procedure (Sluis, P. van der;

Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON

(Spek, A.L. Acta Crystallogr. 1990, A46, C34. PLATON - a multipurpose

crystallographic tool. Utrecht University, Utrecht, The Netherlands).

A total solvent-accessible void volume of 2398.0 A^3^ with a total

electron count of 597 (consistent with four molecules of
solvent dma plus two counter-cations per formula) was
found in the unit cell.
;
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         2264
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                1582
_reflns_number_total             2264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906728k.txt
_cod_data_source_block           NH2BDC-Cd
_cod_database_code               7002482