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_4121071
_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            'C144 H192 N72 Ni14'
_chemical_formula_weight         3753.64
_space_group_IT_number           104
_symmetry_cell_setting           tetragonal
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_symmetry_space_group_name_H-M   'P 4 n c'
_atom_sites_solution_hydrogens   geom
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_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                   16.99570(10)
_cell_length_b                   16.99570(10)
_cell_length_c                   32.7949(5)
_cell_measurement_temperature    100(2)
_cell_volume                     9472.93(16)
_computing_cell_refinement
;       
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 24-05-2012 CrysAlis171 .NET)
(compiled May 24 19:17:45 2013)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 24-05-2012 CrysAlis171 .NET)
(compiled May 24 19:17:45 2013)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 24-05-2012 CrysAlis171 .NET)
(compiled May 24 19:17:45 2013)
;
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17709
_diffrn_reflns_theta_full        74.39
_diffrn_reflns_theta_max         74.39
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    1.946
_exptl_absorpt_correction_T_max  0.6741
_exptl_absorpt_correction_T_min  0.5929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 24-05-2012 CrysAlis171 .NET)
(compiled May 24 19:17:45 2013)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block-like
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7720
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0580P)^2^+0.5410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                5981
_reflns_number_total             7720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4092984_si_002_7.cif
_cod_data_source_block           9
_cod_database_code               4121071