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_4326294
_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 H55 Cu N6, 3(N O3), H2 O'
_chemical_formula_sum            'C25 H57 Cu N9 O10'
_chemical_formula_weight         707.34
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_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
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_cell_angle_beta                 119.174(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   10.7350(6)
_cell_length_c                   19.2966(13)
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_cell_measurement_temperature    293(2)
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_cell_measurement_theta_min      3.0675
_cell_measurement_wavelength     0.71073
_cell_volume                     3435.8(5)
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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_data_reduction
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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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0153858
_diffrn_orient_matrix_UB_12      -0.0604532
_diffrn_orient_matrix_UB_13      0.0141244
_diffrn_orient_matrix_UB_21      -0.0206053
_diffrn_orient_matrix_UB_22      -0.0009273
_diffrn_orient_matrix_UB_23      0.0223228
_diffrn_orient_matrix_UB_31      -0.0341556
_diffrn_orient_matrix_UB_32      -0.0266226
_diffrn_orient_matrix_UB_33      -0.0327872
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.077
_diffrn_reflns_limit_h_max       21
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22796
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.78583
_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    1.367
_exptl_crystal_description       prism
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                4014
_reflns_number_total             6036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201326d_si_002_4.cif
_cod_data_source_block           580pb3
_cod_original_cell_volume        3435.8(4)
_cod_database_code               4326294