A Cubic, 12-Connected, Microporous Metal-Organometallic Phosphate Framework Sustained by Truncated Tetrahedral Nodes
Sayon A. Kumalah Robinson; Marion-Vincent L. Mempin; Amy J. Cairns; K. Travis Holman; Journal of the American Chemical Society 133 (2011) 1634–1637; doi:10.1021/ja108894a

data_4105622
_publ_contact_author_address
;Department of Chemistry
240 Reiss Building
Georgetown University
37th and O st, NW
Washington, DC, 20057
;
_publ_contact_author_email       kth7@georgetown.edu
_publ_contact_author_name        'K. Travis Holman'
_publ_contact_author_phone       '202 687 4027'
_publ_section_title
;
 A Cubic, 12-Connected, Microporous Metal-Organometallic Phosphate
 Framework Sustained by Truncated Tetrahedral Nodes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1634
_journal_page_last               1637
_journal_paper_doi               10.1021/ja108894a
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C84 H84 Co12 F4 Fe6 N2 O55 P4'
_chemical_formula_weight         3243.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           216
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F -4 2 3'
_symmetry_space_group_name_H-M   'F -4 3 m'
_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                   24.1624(9)
_cell_length_b                   24.1624(9)
_cell_length_c                   24.1624(9)
_cell_measurement_reflns_used    4018
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.083
_cell_measurement_theta_min      2.385
_cell_volume                     14106.5(9)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics    'X-SEED, L.Barbour (1999);http://x-seed.net/'
_computing_structure_refinement  'SHELXL-97-2, G. Sheldrick (1997)'
_computing_structure_solution    'SHELXS-97, G. Sheldrick, (1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens SMART 1000 CCD'
_diffrn_measurement_method       '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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3846
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    2.087
_exptl_absorpt_correction_T_max  0.6567
_exptl_absorpt_correction_T_min  0.6343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            'Dark Pink'
_exptl_crystal_density_diffrn    1.5271
_exptl_crystal_description       Cube
_exptl_crystal_F_000             6256
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_platon_squeeze_details
; 
The unit cell contains 3 ethanol molecules and 2 nitrate anions which have been 
treated as a diffuse contribution to the overall scattering without specific 
atom positions by SQUEEZE/PLATON.Since only the major occupancy portion of the 
disordered Cp groups had been modeled by discrete atomic positions the electron
density contributed by the absent Cp ring per formula unit (42 e/SBU)was 
subtracted from the total electron density 179e/SBU outputted by PLATON and the
residual electron contribution was attributed to the solvent and counterion 
molecules.
;
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.38(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0899P)^2^+61.0626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                1144
_reflns_number_total             1258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108894a_si_001.cif
_cod_data_source_block           publication_text
_cod_database_code               4105622