An Unusually Flexible Expanded Hexaamine Cage and Its CuII Complexes: Variable Coordination Modes and Incomplete Encapsulation
Chang-Jin Qin; Lloyd James; Jy D. Chartres; Leighton J. Alcock; Kimberley J. Davis; Anthony C. Willis; Alan M. Sargeson; Paul V. Bernhardt; Stephen F. Ralph; Inorganic Chemistry 50 (2011) 9131–9140; doi:10.1021/ic201326d

data_4326292
_publ_contact_author_address
;
Research School of Chemistry,
The Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' willis@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' Anthony C. Willis '
_publ_contact_author_phone       ' 61 2 6125 4109 '
_publ_section_title
;
 An Unusually Flexible Expanded Hexaamine Cage and Its CuII Complexes:
 Variable Coordination Modes and Incomplete Encapsulation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9131
_journal_page_last               9140
_journal_paper_doi               10.1021/ic201326d
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H58 Cu1 N6, 2(N O3), (H2 O)'
_chemical_formula_sum            'C25 H58 Cu N8 O8'
_chemical_formula_weight         662.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
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_symmetry_space_group_name_Hall  '-P 4bc'
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_cell_measurement_temperature    293(2)
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0696
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0609578
_diffrn_orient_matrix_UB_12      -0.0042306
_diffrn_orient_matrix_UB_13      0.008685
_diffrn_orient_matrix_UB_21      -0.0211144
_diffrn_orient_matrix_UB_22      0.0178191
_diffrn_orient_matrix_UB_23      0.0224095
_diffrn_orient_matrix_UB_31      -0.0102271
_diffrn_orient_matrix_UB_32      -0.062804
_diffrn_orient_matrix_UB_33      0.005736
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1041
_diffrn_reflns_av_unetI/netI     0.305
_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_min       -7
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_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7159
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.72093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
        empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       prism
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.71
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2970
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.709
_refine_ls_R_factor_all          0.2252
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1867
_reflns_number_gt                811
_reflns_number_total             2970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201326d_si_002_2.cif
_cod_data_source_block           505pb1
_cod_original_cell_volume        3379.8(5)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4326292