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_4326291
_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        ' from U of Wollongong'
_chemical_formula_moiety         'C25 H54 N6'
_chemical_formula_sum            'C25 H54 N6'
_chemical_formula_weight         438.74
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-08-20
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record
;
2010-08-20 - Report on C25 H54 N6
             by Anthony C. Willis
             for Steve Ralph

2010-08-20 - passes checkcif tests with minor warnings  
;
_cell_angle_alpha                96.5163(8)
_cell_angle_beta                 112.7701(9)
_cell_angle_gamma                100.3828(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2473(1)
_cell_length_b                   11.4242(2)
_cell_length_c                   12.9246(2)
_cell_measurement_reflns_used    27664
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2.6
_cell_volume                     1343.98(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43381
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.733
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9937
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7826
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.0032468
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.33P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1138
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1138
_reflns_limit_h_max              12
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6649
_reflns_number_total             7826
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.24
_oxford_diffrn_Wilson_scale      0.31
_oxford_refine_ls_r_factor_ref   0.0506
_oxford_refine_ls_scale          1.949(11)
_oxford_reflns_number_all        7826
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '8201153 wol1006'
_cod_data_source_file            ic201326d_si_002_1.cif
_cod_data_source_block           wol1007
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4326291