The Potentially Hexadentate Isomeric Macrocycles trans- and cis-6,13-Diethyl-1,4,8,11-tetraazacyclotetradecane-6,13-diamine and Their Cobalt(III) Complexes: Unexpected Conformational Behavior
Paul V. Bernhardt; Karl A. Byriel; Colin H. L. Kennard; Philip C. Sharpe; Inorganic Chemistry 35 (1996) 2045–2052; doi:10.1021/ic951260y

data_4324061
_publ_contact_author
;
Dr Paul V. Bernhardt
Department of Chemistry
University of Queensland
Brisbane, 4072
Australia
;
_publ_contact_author_email       bernhard@chem.chemistry.uq.oz.au
_publ_contact_author_fax         '+61 7 3365 4273'
_publ_contact_author_phone       '+61 7 3365 4266'
_publ_section_title
;
 The Potentially Hexadentate Isomeric Macrocycles trans- and
 cis-6,13-Diethyl-1,4,8,11-tetraazacyclotetradecane-6,13-diamine and Their
 Cobalt(III) Complexes: Unexpected Conformational Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2045
_journal_page_last               2052
_journal_paper_doi               10.1021/ic951260y
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C14 H42 Cl4 N6 O18'
_chemical_formula_weight         724.34
_chemical_name_systematic
; 
trans-6,13-diammonio-6,13-diethyl-1,8-diaza-4,11-diazoniocyclotetradecane 
perchlorate dihydrate
;
_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_method           SHELXL
_cell_angle_alpha                77.141(6)
_cell_angle_beta                 86.539(9)
_cell_angle_gamma                86.465(9)
_cell_formula_units_Z            2
_cell_length_a                   7.840(1)
_cell_length_b                   13.6206(9)
_cell_length_c                   14.246(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     1478.6(2)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4 microvax controlled'
_computing_data_reduction        'DIFDAT, XTAL3.2'
_computing_molecular_graphics    PLATON
_computing_publication_material  SHELXL-93
_computing_structure_refinement  SHELXL-93
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      296
_diffrn_measurement_device       'Enraf-Nonius CAD4-circle diffractometer'
_diffrn_measurement_method       '2\q/\w scan mode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10388
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  1.092
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       needle
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         5194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_obs          0.0349
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.9253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0970
_refine_ls_wR_factor_obs         0.0933
_reflns_number_observed          4624
_reflns_number_total             5194
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951260y_1.cif
_cod_data_source_block           906pcs3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.9253P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.9253P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4324061
_cod_database_fobs_code          4324061