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_4324062
_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 H34 Cl3 Co N6 O12'
_chemical_formula_weight         643.75
_chemical_name_systematic
;
trans-6,13-diethyl-1,4,8,11-tetraazacyclotetradecane-6,13-diamine 
cobalt(III) perchlorate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.96(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.461(6)
_cell_length_b                   11.580(2)
_cell_length_c                   15.865(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     2464.0(14)
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2254
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  1.767
_exptl_absorpt_correction_T_min  1.012
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_obs          0.0586
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+2.9964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1706
_refine_ls_wR_factor_obs         0.1543
_reflns_number_observed          1689
_reflns_number_total             2165
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951260y_2.cif
_cod_data_source_block           891pcs2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+2.9964P] 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^)+(0.1276P)^2^+2.9964P] 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               4324062
_cod_database_fobs_code          4324062