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_4121069
_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            'C2.8 H3.73 Br0.08 N1.4 Ni0.27 O0.06'
_chemical_formula_weight         80.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           104
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_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            103
_cell_length_a                   17.2136(4)
_cell_length_b                   17.2136(4)
_cell_length_c                   32.7939(19)
_cell_measurement_temperature    293(2)
_cell_volume                     9717.1(6)
_computing_cell_refinement
;       
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 25-02-2013 CrysAlis171 .NET)
(compiled Feb 25 10:27:04 2013)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 25-02-2013 CrysAlis171 .NET)
(compiled Feb 25 10:27:04 2013)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 25-02-2013 CrysAlis171 .NET)
(compiled Feb 25 10:27:04 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      293(2)
_diffrn_detector_area_resol_mean 10.4098
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15373
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    2.887
_exptl_absorpt_correction_T_max  0.589
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 25-02-2013 CrysAlis171 .NET)
(compiled Feb 25 10:27:04 2013)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block-like
_exptl_crystal_F_000             4232
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.048
_refine_diff_density_min         -1.959
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         5889
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1555P)^2^+1.2899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.1997
_reflns_number_gt                5287
_reflns_number_total             5889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4092984_si_002_5.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C2.80 H3.73 Br0.08 N1.40 Ni0.27 O0.06'
_cod_database_code               4121069