Charge effect of foreign metal ions and the crystal growth process in hybridized metal-organic frameworks
Woo Ram Lee; Dae Won Ryu; Won Ju Phang; Ji Hye Park; Chang Seop Hong; Chem.Commun. 48 (2012) 10847–; doi:10.1039/c2cc35526d

data_7108523
_publ_section_title
;
 Charge effect of foreign metal ions and the crystal growth process in
 hybridized metal-organic frameworks
;
_journal_name_full               Chem.Commun.
_journal_page_first              10847
_journal_paper_doi               10.1039/c2cc35526d
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C258 H384 N13.33 O129 P8 Zn15'
_chemical_formula_weight         6964.76
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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            3
_cell_length_a                   34.340(3)
_cell_length_b                   34.340(3)
_cell_length_c                   19.451(2)
_cell_measurement_reflns_used    2455
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.2715
_cell_measurement_theta_min      3.7745
_cell_volume                     19864(3)
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_collection       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scan'
_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  0.0935
_diffrn_reflns_av_sigmaI/netI    0.1439
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27880
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  0.8687
_exptl_absorpt_correction_T_min  0.7426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10882
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The contributions of some 1259 electrons were removed from the unit-cell contents.
The oxygen (O4) atom is at a site with -3 symmetry and there are six Zn(II)2.5 formula units in the unit cell.
Therefore, this could/might correspond with the removal of solvent
such as 5(DMF) and 1(H2O) [some 210 electrons] from the Zn(II)2.5 formula unit.
;
_refine_diff_density_max         1.350
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         10904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1166P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2382
_reflns_number_gt                4379
_reflns_number_total             10904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35526d.txt
_cod_data_source_block           squeezed
_cod_original_cell_volume        19865(4)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7108523