A cobalt(III) compound of a 13-membered cyclic tetraamine: <i>trans</i>-(12,12-dimethyl-1,4,7,10-tetraazacyclotetradecane)diisothiocyanatocobalt(III) tetraisothiocyanatozinc(II) ethanol solvate
Neil F. Curtis; Kelly Flood; Ward T. Robinson; Acta Crystallographica Section C 62 (2006) m78–m80; doi:10.1107/S0108270105042940

data_2014354
_publ_section_title
;A cobalt(III) compound of a 13-membered cyclic tetraamine:
 <i>trans</i>-(12,12-dimethyl-1,4,7,10-tetraazacyclotetradecane)diisothiocyanatocobalt(III)
 tetraisothiocyanatozinc(II) ethanol solvate
;
_journal_coeditor_code           HJ1078
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m78
_journal_page_last               m80
_journal_paper_doi               10.1107/S0108270105042940
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Co (C11 H26 N4) (N C S)2]2 [Zn (N C S)4] , C2 H6 O'
_chemical_formula_moiety
'2C13 H26 Co N6 S2 + , C4 N4 S4 Zn 2- , C2 H6 O'
_chemical_formula_sum            'C32 H58 Co2 N16 O S8 Zn'
_chemical_formula_weight         1122.66
_chemical_name_systematic
;
trans-(12,12-dimethyl-1,4,7,10-
tetraazacyclotetradecane)diisothiocyanatocobalt(III)
tetraisothiocyanatozinc(II) ethanol solvate
;
_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           SHELXL97
_cell_angle_alpha                70.511(2)
_cell_angle_beta                 82.199(2)
_cell_angle_gamma                71.989(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9776(6)
_cell_length_b                   14.0647(8)
_cell_length_c                   19.5860(10)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      32.3
_cell_measurement_theta_min      1.1
_cell_volume                     2462.5(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997 or Siemens, 1995?)'
_computing_data_reduction        'SAINT (Bruker, 1997 or Siemens, 1995?)'
_computing_molecular_graphics    'ORTEP3.2 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51668
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.31
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_correction_T_min  0.3955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Version 2.03; Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.610
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         14587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0375P)^2^+1.5995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                13265
_reflns_number_total             14587
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hj1078.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (25 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (25
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (38 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2014354
_cod_database_fobs_code          2014354