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_4326293
_publ_contact_author_address
;
Research School of Chemistry,
The Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' Anthony.Willis@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        local
_chemical_formula_moiety         'C25 H54 Cu N6 2+,  S2 O6 2-'
_chemical_formula_sum            'C25 H54 Cu N6 O6 S2'
_chemical_formula_weight         662.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2010-11-25
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
1997-04-08 original report 
2011-01-10 edit cif from that
;
_cell_angle_alpha                90
_cell_angle_beta                 90.68(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.527(1)
_cell_length_b                   15.585(2)
_cell_length_c                   19.257(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      19.3
_cell_volume                     3159.1(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_diffrn_ambient_temperature      296.2
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.08703
_diffrn_orient_matrix_UB_12      0.02103
_diffrn_orient_matrix_UB_13      0.01256
_diffrn_orient_matrix_UB_21      -0.03384
_diffrn_orient_matrix_UB_22      0.05967
_diffrn_orient_matrix_UB_23      0.00462
_diffrn_orient_matrix_UB_31      -0.01749
_diffrn_orient_matrix_UB_32      -0.01071
_diffrn_orient_matrix_UB_33      0.05018
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.01654
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6006
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        -0.94
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       rod
_exptl_crystal_F_000             1420.00
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.472
_refine_ls_goodness_of_fit_gt    1.647
_refine_ls_goodness_of_fit_ref   1.647
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     379
_refine_ls_number_reflns         3678
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.0410
_refine_ls_shift/su_mean         0.0040
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0390
_refine_ls_wR_factor_gt          0.0347
_refine_ls_wR_factor_ref         0.0347
_reflns_number_gt                3678
_reflns_number_total             5594
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201326d_si_002_3.cif
_cod_data_source_block           cjq18
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C25 H54 Cu N6 O6 S2 '
_cod_database_code               4326293