Polyhedral Metal-Imidazolate Cages: Control of Self-Assembly and Cage to Cage Transformation
Xiao-Ping Zhou; Yuan Wu; Dan Li; Journal of the American Chemical Society 135 (2013) 16062–16065; doi:10.1021/ja4092984

data_4121072
_publ_section_title
;
 Polyhedral Metal-Imidazolate Cages: Control of Self-Assembly and Cage to
 Cage Transformation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16062
_journal_page_last               16065
_journal_paper_doi               10.1021/ja4092984
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C312 H336 N72 Ni14 O24'
_chemical_formula_weight         6300.47
_space_group_IT_number           90
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4ab 2ab'
_symmetry_space_group_name_H-M   'P 4 21 2'
_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            2
_cell_length_a                   26.9825(2)
_cell_length_b                   26.9825(2)
_cell_length_c                   24.9570(3)
_cell_measurement_temperature    100(2)
_cell_volume                     18170.1(3)
_computing_cell_refinement
;       
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 24-10-2012 CrysAlis171 .NET)
(compiled Oct 24 21:31:26 2012)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 24-10-2012 CrysAlis171 .NET)
(compiled Oct 24 21:31:26 2012)
;
_computing_data_reduction
;       
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 24-10-2012 CrysAlis171 .NET)
(compiled Oct 24 21:31:26 2012)
;
_computing_molecular_graphics    Olex-2
_computing_publication_material  Olex-2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4098
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32566
_diffrn_reflns_theta_full        63.00
_diffrn_reflns_theta_max         63.00
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.8949
_exptl_absorpt_correction_T_min  0.8333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 24-10-2012 CrysAlis171 .NET)
(compiled Oct 24 21:31:26 2012)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       block-like
_exptl_crystal_F_000             6592
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
;
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         13814
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0756
_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^)+(0.1230P)^2^+12.3643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1899
_refine_ls_wR_factor_ref         0.2058
_reflns_number_gt                10650
_reflns_number_total             13814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4092984_si_002_8.cif
_cod_data_source_block           12
_cod_database_code               4121072