#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/48/2214801.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214801
loop_
_publ_author_name
'Kropidłowska, Anna'
'Chojnacki, Jarosław'
'Gołaszewska, Jolanta'
'Paliwoda, Damian'
'Becker, Barbara'
_publ_section_title
;
 Tris(4-morpholinecarbodithioato-κ²S,S')cobalt(III)
;
_journal_coeditor_code           LX2018
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2117
_journal_page_last               m2117
_journal_paper_doi               10.1107/S160053680703276X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Co (C5 H8 N O S2)3]'
_chemical_formula_moiety         'C15 H24 Co1 N3 O3 S6'
_chemical_formula_sum            'C15 H24 Co N3 O3 S6'
_chemical_formula_weight         545.66
_chemical_name_systematic
;
Tris(4-morpholinecarbodithioato-κ²S,S')cobalt(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.006(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1952(6)
_cell_length_b                   11.4668(5)
_cell_length_c                   15.7281(9)
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.4864
_cell_measurement_theta_min      2.367
_cell_volume                     2336.0(2)
_computing_cell_refinement       'CrysAlis RED'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae et al.,
2006)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Oxford Diffraction KM4 CCD area-detector'
_diffrn_measurement_device_type  'Oxford Diffraction KM4 CCD area-detector'
_diffrn_measurement_method       'ω scans, 0.75 deg width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12971
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis RED (Oxford Diffraction, 2006); analytical numerical
absorption correction using a multifaceted crystal model (Clark & Reid,
1995)]
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.1877
_exptl_crystal_size_mid          0.0986
_exptl_crystal_size_min          0.0212
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.816
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0719P)²+4.281P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.122
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                4094
_reflns_number_total             4538
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lx2018.cif
_cod_data_source_block           I
_cod_database_code               2214801
_cod_database_fobs_code          2214801
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Co Co1 0.26983(3) 0.01485(4) 0.26399(3) 0.01532(14) Uani d . 1
S S1 0.42699(6) 0.10412(7) 0.28576(5) 0.0203(2) Uani d . 1
S S2 0.30882(6) 0.03786(7) 0.40951(5) 0.01715(19) Uani d . 1
S S3 0.33634(6) -0.16687(7) 0.25782(5) 0.01816(19) Uani d . 1
S S4 0.13436(6) -0.10359(7) 0.27236(5) 0.01796(19) Uani d . 1
S S5 0.23133(6) 0.03742(7) 0.11798(5) 0.01843(19) Uani d . 1
S S6 0.17989(6) 0.18432(7) 0.24632(5) 0.01834(19) Uani d . 1
N N1 0.4846(2) 0.1614(3) 0.45449(17) 0.0203(6) Uani d . 1
N N2 0.1923(2) -0.3293(2) 0.27148(19) 0.0216(6) Uani d . 1
N N3 0.1270(2) 0.2387(2) 0.07649(17) 0.0221(6) Uani d . 1
O O1 0.5547(2) 0.3653(2) 0.54704(17) 0.0362(6) Uani d . 1
O O2 0.1546(2) -0.5539(2) 0.33120(16) 0.0276(5) Uani d . 1
O O3 -0.0211(2) 0.3479(2) -0.05188(15) 0.0292(6) Uani d . 1
C C1 0.4184(2) 0.1095(3) 0.3928(2) 0.0171(6) Uani d . 1
C C2 0.5761(3) 0.2238(3) 0.4379(2) 0.0246(7) Uani d . 1
H H2A 0.5812 0.2157 0.3762 0.032 Uiso calc R 1
H H2B 0.6392 0.1902 0.4737 0.032 Uiso calc R 1
C C3 0.5668(3) 0.3514(3) 0.4601(2) 0.0333(9) Uani d . 1
H H3A 0.6294 0.3936 0.4513 0.043 Uiso calc R 1
H H3B 0.5066 0.3859 0.4209 0.043 Uiso calc R 1
C C4 0.4636(3) 0.3081(3) 0.5611(2) 0.0305(8) Uani d . 1
H H4A 0.4028 0.3427 0.5228 0.04 Uiso calc R 1
H H4B 0.4558 0.3202 0.6218 0.04 Uiso calc R 1
C C5 0.4676(3) 0.1783(3) 0.5430(2) 0.0231(7) Uani d . 1
H H5A 0.5243 0.1417 0.5847 0.03 Uiso calc R 1
H H5B 0.4018 0.1411 0.5496 0.03 Uiso calc R 1
C C6 0.2173(2) -0.2175(3) 0.2675(2) 0.0186(6) Uani d . 1
C C7 0.2634(3) -0.4253(3) 0.2633(2) 0.0267(8) Uani d . 1
H H7A 0.3347 -0.3949 0.2702 0.035 Uiso calc R 1
H H7B 0.2445 -0.4606 0.2049 0.035 Uiso calc R 1
C C8 0.2581(3) -0.5172(3) 0.3318(3) 0.0291(8) Uani d . 1
H H8A 0.3 -0.5855 0.3215 0.038 Uiso calc R 1
H H8B 0.2881 -0.4851 0.3896 0.038 Uiso calc R 1
C C9 0.0937(3) -0.4574(3) 0.3478(2) 0.0243(7) Uani d . 1
H H9A 0.1245 -0.4219 0.4042 0.032 Uiso calc R 1
H H9B 0.0233 -0.4844 0.351 0.032 Uiso calc R 1
C C10 0.0878(2) -0.3671(3) 0.2769(2) 0.0215(7) Uani d . 1
H H10A 0.0534 -0.4008 0.2209 0.028 Uiso calc R 1
H H10B 0.0466 -0.2994 0.2898 0.028 Uiso calc R 1
C C11 0.1718(2) 0.1661(3) 0.1371(2) 0.0179(6) Uani d . 1
C C12 0.1283(3) 0.2207(3) -0.0155(2) 0.0251(7) Uani d . 1
H H12A 0.1536 0.1412 -0.0245 0.033 Uiso calc R 1
H H12B 0.1755 0.2776 -0.0349 0.033 Uiso calc R 1
C C13 0.0202(3) 0.2361(3) -0.0674(2) 0.0263(7) Uani d . 1
H H13A 0.0216 0.2282 -0.1299 0.034 Uiso calc R 1
H H13B -0.025 0.1742 -0.0516 0.034 Uiso calc R 1
C C14 -0.0276(3) 0.3579(3) 0.0376(2) 0.0256(7) Uani d . 1
H H14A -0.0726 0.2953 0.0529 0.033 Uiso calc R 1
H H14B -0.059 0.4338 0.0476 0.033 Uiso calc R 1
C C15 0.0785(3) 0.3487(3) 0.0951(2) 0.0243(7) Uani d . 1
H H15A 0.1219 0.4154 0.0839 0.032 Uiso calc R 1
H H15B 0.072 0.351 0.1567 0.032 Uiso calc R 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
S2 Co1 S6 92.10(3)
S2 Co1 S4 92.33(3)
S6 Co1 S4 96.91(3)
S2 Co1 S5 166.76(4)
S6 Co1 S5 76.55(3)
S4 Co1 S5 95.75(3)
S2 Co1 S3 97.76(3)
S6 Co1 S3 168.36(3)
S4 Co1 S3 76.61(3)
S5 Co1 S3 94.31(3)
S2 Co1 S1 76.77(3)
S6 Co1 S1 94.22(3)
S4 Co1 S1 164.70(3)
S5 Co1 S1 97.02(3)
S3 Co1 S1 94.05(3)
C1 S1 Co1 86.30(10)
C1 S2 Co1 86.40(10)
C6 S3 Co1 86.50(10)
C6 S4 Co1 86.40(10)
C11 S5 Co1 86.70(10)
C11 S6 Co1 87.10(10)
C1 N1 C5 124.0(3)
C1 N1 C2 122.8(3)
C5 N1 C2 112.6(3)
C6 N2 C10 122.2(3)
C6 N2 C7 123.4(3)
C10 N2 C7 114.1(3)
C11 N3 C12 122.5(3)
C11 N3 C15 123.4(3)
C12 N3 C15 113.9(3)
C3 O1 C4 110.6(3)
C9 O2 C8 110.1(3)
C14 O3 C13 109.6(2)
N1 C1 S1 125.6(2)
N1 C1 S2 124.1(2)
S1 C1 S2 110.33(17)
N1 C2 C3 108.9(3)
N1 C2 H2A 109.9
C3 C2 H2A 109.9
N1 C2 H2B 109.9
C3 C2 H2B 109.9
H2A C2 H2B 108.3
O1 C3 C2 111.2(3)
O1 C3 H3A 109.4
C2 C3 H3A 109.4
O1 C3 H3B 109.4
C2 C3 H3B 109.4
H3A C3 H3B 108
O1 C4 C5 111.3(3)
O1 C4 H4A 109.4
C5 C4 H4A 109.4
O1 C4 H4B 109.4
C5 C4 H4B 109.4
H4A C4 H4B 108
N1 C5 C4 109.0(3)
N1 C5 H5A 109.9
C4 C5 H5A 109.9
N1 C5 H5B 109.9
C4 C5 H5B 109.9
H5A C5 H5B 108.3
N2 C6 S3 124.9(3)
N2 C6 S4 124.5(3)
S3 C6 S4 110.5(2)
N2 C7 C8 110.0(3)
N2 C7 H7A 109.7
C8 C7 H7A 109.7
N2 C7 H7B 109.7
C8 C7 H7B 109.7
H7A C7 H7B 108.2
O2 C8 C7 111.9(3)
O2 C8 H8A 109.2
C7 C8 H8A 109.2
O2 C8 H8B 109.2
C7 C8 H8B 109.2
H8A C8 H8B 107.9
O2 C9 C10 110.5(3)
O2 C9 H9A 109.6
C10 C9 H9A 109.6
O2 C9 H9B 109.6
C10 C9 H9B 109.6
H9A C9 H9B 108.1
N2 C10 C9 109.2(3)
N2 C10 H10A 109.8
C9 C10 H10A 109.8
N2 C10 H10B 109.8
C9 C10 H10B 109.8
H10A C10 H10B 108.3
N3 C11 S6 125.6(3)
N3 C11 S5 124.8(2)
S6 C11 S5 109.6(2)
N3 C12 C13 109.2(3)
N3 C12 H12A 109.8
C13 C12 H12A 109.8
N3 C12 H12B 109.8
C13 C12 H12B 109.8
H12A C12 H12B 108.3
O3 C13 C12 111.3(3)
O3 C13 H13A 109.4
C12 C13 H13A 109.4
O3 C13 H13B 109.4
C12 C13 H13B 109.4
H13A C13 H13B 108
O3 C14 C15 111.0(3)
O3 C14 H14A 109.4
C15 C14 H14A 109.4
O3 C14 H14B 109.4
C15 C14 H14B 109.4
H14A C14 H14B 108
N3 C15 C14 109.1(3)
N3 C15 H15A 109.9
C14 C15 H15A 109.9
N3 C15 H15B 109.9
C14 C15 H15B 109.9
H15A C15 H15B 108.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 S2 2.2634(8)
Co1 S6 2.2663(9)
Co1 S4 2.2688(9)
Co1 S5 2.2702(8)
Co1 S3 2.2703(9)
Co1 S1 2.2790(9)
S1 C1 1.710(3)
S2 C1 1.726(3)
S3 C6 1.708(3)
S4 C6 1.715(3)
S5 C11 1.725(3)
S6 C11 1.713(3)
N1 C1 1.317(4)
N1 C5 1.465(4)
N1 C2 1.468(4)
N2 C6 1.329(4)
N2 C10 1.464(4)
N2 C7 1.468(4)
N3 C11 1.318(4)
N3 C12 1.465(4)
N3 C15 1.469(4)
O1 C3 1.415(5)
O1 C4 1.423(5)
O2 C9 1.420(4)
O2 C8 1.428(4)
O3 C14 1.430(4)
O3 C13 1.432(4)
C2 C3 1.516(5)
C2 H2A 0.99
C2 H2B 0.99
C3 H3A 0.99
C3 H3B 0.99
C4 C5 1.518(5)
C4 H4A 0.99
C4 H4B 0.99
C5 H5A 0.99
C5 H5B 0.99
C7 C8 1.519(5)
C7 H7A 0.99
C7 H7B 0.99
C8 H8A 0.99
C8 H8B 0.99
C9 C10 1.512(5)
C9 H9A 0.99
C9 H9B 0.99
C10 H10A 0.99
C10 H10B 0.99
C12 C13 1.513(5)
C12 H12A 0.99
C12 H12B 0.99
C13 H13A 0.99
C13 H13B 0.99
C14 C15 1.518(5)
C14 H14A 0.99
C14 H14B 0.99
C15 H15A 0.99
C15 H15B 0.99
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
S2 Co1 S1 C1 -3.29(11)
S6 Co1 S1 C1 87.88(11)
S4 Co1 S1 C1 -48.75(18)
S5 Co1 S1 C1 164.83(11)
S3 Co1 S1 C1 -100.32(11)
S6 Co1 S2 C1 -90.58(11)
S4 Co1 S2 C1 172.41(11)
S5 Co1 S2 C1 -59.94(18)
S3 Co1 S2 C1 95.61(11)
S1 Co1 S2 C1 3.26(11)
S2 Co1 S3 C6 89.61(11)
S6 Co1 S3 C6 -58.1(2)
S4 Co1 S3 C6 -0.94(10)
S5 Co1 S3 C6 -95.84(11)
S1 Co1 S3 C6 166.79(11)
S2 Co1 S4 C6 -96.49(11)
S6 Co1 S4 C6 171.11(10)
S5 Co1 S4 C6 94.01(11)
S3 Co1 S4 C6 0.94(10)
S1 Co1 S4 C6 -52.51(17)
S2 Co1 S5 C11 -30.55(18)
S6 Co1 S5 C11 1.03(10)
S4 Co1 S5 C11 96.79(11)
S3 Co1 S5 C11 173.73(11)
S1 Co1 S5 C11 -91.64(11)
S2 Co1 S6 C11 172.07(11)
S4 Co1 S6 C11 -95.33(11)
S5 Co1 S6 C11 -1.04(11)
S3 Co1 S6 C11 -39.9(2)
S1 Co1 S6 C11 95.19(11)
C5 N1 C1 S1 171.1(3)
C2 N1 C1 S1 0.6(5)
C5 N1 C1 S2 -8.2(5)
C2 N1 C1 S2 -178.7(3)
Co1 S1 C1 N1 -174.9(3)
Co1 S1 C1 S2 4.48(15)
Co1 S2 C1 N1 174.9(3)
Co1 S2 C1 S1 -4.51(15)
C1 N1 C2 C3 116.9(3)
C5 N1 C2 C3 -54.6(4)
C4 O1 C3 C2 -60.6(4)
N1 C2 C3 O1 56.9(4)
C3 O1 C4 C5 60.2(4)
C1 N1 C5 C4 -117.1(3)
C2 N1 C5 C4 54.2(4)
O1 C4 C5 N1 -56.1(4)
C10 N2 C6 S3 -178.0(2)
C7 N2 C6 S3 -3.5(5)
C10 N2 C6 S4 2.7(5)
C7 N2 C6 S4 177.2(2)
Co1 S3 C6 N2 -178.1(3)
Co1 S3 C6 S4 1.30(14)
Co1 S4 C6 N2 178.1(3)
Co1 S4 C6 S3 -1.30(14)
C6 N2 C7 C8 135.6(3)
C10 N2 C7 C8 -49.5(4)
C9 O2 C8 C7 -60.1(4)
N2 C7 C8 O2 52.4(4)
C8 O2 C9 C10 62.8(3)
C6 N2 C10 C9 -132.7(3)
C7 N2 C10 C9 52.3(4)
O2 C9 C10 N2 -58.1(3)
C12 N3 C11 S6 176.3(3)
C15 N3 C11 S6 1.2(5)
C12 N3 C11 S5 -3.8(5)
C15 N3 C11 S5 -178.9(3)
Co1 S6 C11 N3 -178.7(3)
Co1 S6 C11 S5 1.41(14)
Co1 S5 C11 N3 178.7(3)
Co1 S5 C11 S6 -1.41(14)
C11 N3 C12 C13 132.2(3)
C15 N3 C12 C13 -52.3(4)
C14 O3 C13 C12 -61.6(4)
N3 C12 C13 O3 56.1(4)
C13 O3 C14 C15 61.6(4)
C11 N3 C15 C14 -132.2(3)
C12 N3 C15 C14 52.3(4)
O3 C14 C15 N3 -56.1(4)
