Crown Ether Appended Cyclam Receptors for Cationic Guests
Paul V. Bernhardt; Elizabeth J. Hayes; Inorganic Chemistry 41 (2002) 2892–2902; doi:10.1021/ic011232h

data_4318025
_publ_section_title
;
 Crown Ether Appended Cyclam Receptors for Cationic Guests
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2892
_journal_page_last               2902
_journal_paper_doi               10.1021/ic011232h
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29 H54 Cl3 Co1 N6018'
_chemical_formula_structural     'C29 H54 N6018 CO CL3'
_chemical_formula_sum            'C29 H60 Cl3 Co N6 Na O21.5'
_chemical_formula_weight         1025.1
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-10-04T15:38:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                104.520(10)
_cell_angle_beta                 97.42(2)
_cell_angle_gamma                106.05(2)
_cell_formula_units_Z            2
_cell_length_a                   10.755(5)
_cell_length_b                   10.948(2)
_cell_length_c                   20.690(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_measurement_wavelength     0.71073
_cell_volume                     2214.3(12)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
    x-axis points to radiation source
    the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.49392E-1
_diffrn_orient_matrix_UB_12      0.17027E-1
_diffrn_orient_matrix_UB_13      0.47457E-1
_diffrn_orient_matrix_UB_21      -0.85858E-1
_diffrn_orient_matrix_UB_22      -0.26978E-1
_diffrn_orient_matrix_UB_23      0.14745E-1
_diffrn_orient_matrix_UB_31      -0.179E-3
_diffrn_orient_matrix_UB_32      -0.94431E-1
_diffrn_orient_matrix_UB_33      -0.11864E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1078
_diffrn_reflns_av_unetI/netI     0.2841
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8214
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        8
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.9347
_exptl_absorpt_correction_T_min  0.6224
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
          Number of psi-scan sets used was   4
          Theta correction was applied.
          Averaged transmission function was used.
          No Fourier smoothing was applied.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         7759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.3031
_refine_ls_R_factor_gt           0.0978
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2371
_refine_ls_wR_factor_ref         0.3388
_reflns_number_gt                2372
_reflns_number_total             7759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011232h_5.cif
_cod_data_source_block           eh36172
_cod_original_formula_sum        'C29 H60 Cl3 Co N6 Na O21.50'
_cod_database_code               4318025
_exptl_absorpt_factor_mur        0.064
_exptl_absorpt_correction_t_ave  0.7844
_diffrn_standards_decay_corr_max 1.082
_diffrn_standards_decay_corr_min 0.878