Cyanocobalt(III) complexes of penta- and tetradentate-coordinated macrocyclic hexaamines
Paul V. Bernhardt; Nathan L. Kilah; Acta Crystallographica Section C 61 (2005) m245–m249; doi:10.1107/S0108270105009261

data_2014870
_publ_section_title
;
 Cyanocobalt(III) complexes of penta- and tetradentate-coordinated
 macrocyclic hexaamines
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m245
_journal_page_last               m249
_journal_paper_doi               10.1107/S0108270105009261
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'[Co (C14 H32 N8)] [Co (C14 H30 N8)] (Cl O4)3 , 4H2 O'
_chemical_formula_moiety
'C14 H32 Co N8 3+ , C14 H30 Co N8 + , 4Cl O4 - , 4H2 O'
_chemical_formula_sum            'C28 H70 Cl4 Co2 N16 O20'
_chemical_formula_weight         1210.66
_chemical_name_systematic
;
trans-Dicyano(trans-6,13-dimethyl-1,4,8,11-tetraazacyclotetradecane-
6,13-diamine)cobalt(III) trans-dicyano(trans-6,13-dimethyl-
1,4,8,11-tetraazacyclotetradecane-6,13-diaminium)cobalt(III) tetraperchlorate
tetrahydrate
;
_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_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.805(6)
_cell_angle_beta                 82.909(7)
_cell_angle_gamma                81.743(5)
_cell_formula_units_Z            1
_cell_length_a                   9.0697(3)
_cell_length_b                   10.5362(5)
_cell_length_c                   13.3674(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      13.814
_cell_measurement_theta_min      11.215
_cell_volume                     1254.21(11)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2003)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'non-profiled \w/2\q'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4719
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.8055
_exptl_absorpt_correction_T_min  0.7909
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details
;
(North <i>et al.</i>, 1968)         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            yellow
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.956
_refine_ls_extinction_coef       0.044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4412
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.09P)^2^+2.931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1657
_reflns_number_gt                3690
_reflns_number_total             4412
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rb1000.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2014870
_cod_database_fobs_code          2014870