Long tailed cage amines: Synthesis, metal complexation, and structure.
Dittrich, Birger; Harrowfield, Jack M.; Koutsantonis, George A.; Nealon, Gareth L.; Skelton, Brian W.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 3433–3448; doi:10.1039/b921930g

data_7024826
_publ_section_title
;
 Long tailed cage amines: Synthesis, metal complexation, and structure.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3433
_journal_page_last               3448
_journal_paper_doi               10.1039/b921930g
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C28 H61 Cu N7, 2(Cl O4)'
_chemical_formula_sum            'C28 H61 Cl2 Cu N7 O8'
_chemical_formula_weight         758.28
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-06-29T18:38:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                91.86(2)
_cell_angle_beta                 99.60(2)
_cell_angle_gamma                119.65(2)
_cell_formula_units_Z            4
_cell_length_a                   8.803(3)
_cell_length_b                   17.759(4)
_cell_length_c                   27.012(10)
_cell_measurement_reflns_used    9187
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.0207
_cell_measurement_theta_min      2.8806
_cell_volume                     3586(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type
;
Oxford Diffraction Gemini diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0456610651
_diffrn_orient_matrix_UB_12      -0.0226688768
_diffrn_orient_matrix_UB_13      0.0453882387
_diffrn_orient_matrix_UB_21      -0.0663668707
_diffrn_orient_matrix_UB_22      -0.0928942749
_diffrn_orient_matrix_UB_23      -0.0277195121
_diffrn_orient_matrix_UB_31      0.0637959203
_diffrn_orient_matrix_UB_32      -0.0308170348
_diffrn_orient_matrix_UB_33      0.0243134025
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38793
_diffrn_reflns_theta_full        66.04
_diffrn_reflns_theta_max         66.04
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    2.694
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.864
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         12163
_refine_ls_number_restraints     488
_refine_ls_restrained_S_all      1.978
_refine_ls_R_factor_all          0.2142
_refine_ls_R_factor_gt           0.184
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3883
_refine_ls_wR_factor_ref         0.4259
_reflns_number_gt                7178
_reflns_number_total             12163
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b921930g.txt
_cod_data_source_block           gk165
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               7024826
_diffrn_reflns_twin_matrix
;
1.00 0.00 0.00 -2.00 -1.00 0.00 -1.00 0.00 -1.00
;
_refine_ls_twin_fraction         0.37