#------------------------------------------------------------------------------
#$Date: 2017-03-05 07:54:38 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193922 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/07/2020726.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_2020726
loop_
_publ_author_name
'Stinghen, Danilo'
'Rüdiger, André Luis'
'Giese, Siddhartha O. K.'
'Nunes, Giovana G.'
'Soares, Jaísa F.'
'Hughes, David L.'
_publ_section_title
;
 Cobalt(II) chloride adducts with acetonitrile, propan-2-ol and
 tetrahydrofuran: considerations on nuclearity, reactivity and synthetic
 applications
;
_journal_coeditor_code           KY3112
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              104
_journal_page_last               114
_journal_paper_doi               10.1107/S2053229617000705
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac
'[Co (C2 H3 N)4 (C4 H8 O)2], 2[Co Cl3 (C2 H3 N)]'
_chemical_formula_moiety         'C16 H28 Co N4 O2, 2(C2 H3 Cl3 Co N)'
_chemical_formula_structural
'[Co (C2 H3 N)4 (C4 H8 O)2], 2[Co Cl3 (C2 H3 N)]'
_chemical_formula_sum            'C20 H34 Cl6 Co3 N6 O2'
_chemical_formula_weight         780.02
_chemical_name_common            'Cobalt complex, 1'
_chemical_name_systematic
;
Tetrakis(acetonitrile-κN)bis(tetrahydrofuran-κO)cobalt(II)
bis[(acetonitrile-κN)trichloridocobaltate(II)]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                99.665(3)
_cell_angle_beta                 104.290(3)
_cell_angle_gamma                93.968(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7669(6)
_cell_length_b                   9.1516(6)
_cell_length_c                   12.4114(9)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.72
_cell_volume                     837.10(11)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
ORTEP (Johnson, 1976) and ORTEP-3 (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b) and WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.589
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            'translucent intense blue'
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             395
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0242P)²+0.4147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                3389
_reflns_number_total             3836
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ky3112sup1.cif
_cod_data_source_block           compound-1
_cod_original_cell_volume        837.09(11)
_cod_database_code               2020726
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.833
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.5000 0.0000 0.5000 0.01311(6) Uani d 1 A .
O O1 0.64865(14) 0.08899(11) 0.66575(8) 0.0191(2) Uani d 1 . .
C C10A 0.7311(3) 0.0011(2) 0.74676(16) 0.0485(6) Uani d 0.374(14) A 1
H H10A 0.6482 -0.0883 0.7420 0.058 Uiso calc 0.374(14) A 1
H H10B 0.8415 -0.0324 0.7296 0.058 Uiso calc 0.374(14) A 1
C C11A 0.7731(15) 0.0898(8) 0.8578(6) 0.0323(17) Uani d 0.374(14) A 1
H H11A 0.8950 0.0775 0.9010 0.039 Uiso calc 0.374(14) A 1
H H11B 0.6868 0.0601 0.8993 0.039 Uiso calc 0.374(14) A 1
C C12A 0.7619(2) 0.2510(2) 0.84281(15) 0.0333(4) Uani d 0.374(14) A 1
H H12A 0.7114 0.3073 0.9008 0.040 Uiso calc 0.374(14) A 1
H H12B 0.8813 0.3015 0.8481 0.040 Uiso calc 0.374(14) A 1
C C10B 0.7311(3) 0.0011(2) 0.74676(16) 0.0485(6) Uani d 0.626(14) A 2
H H10C 0.8044 -0.0690 0.7139 0.058 Uiso calc 0.626(14) A 2
H H10D 0.6391 -0.0566 0.7705 0.058 Uiso calc 0.626(14) A 2
C C11B 0.8468(10) 0.1131(6) 0.8458(4) 0.0402(14) Uani d 0.626(14) A 2
H H11C 0.8512 0.0788 0.9179 0.048 Uiso calc 0.626(14) A 2
H H11D 0.9702 0.1285 0.8379 0.048 Uiso calc 0.626(14) A 2
C C12B 0.7619(2) 0.2510(2) 0.84281(15) 0.0333(4) Uani d 0.626(14) A 2
H H12C 0.8539 0.3379 0.8595 0.040 Uiso calc 0.626(14) A 2
H H12D 0.6927 0.2647 0.9002 0.040 Uiso calc 0.626(14) A 2
C C13 0.6404(2) 0.23802(17) 0.72689(14) 0.0299(4) Uani d 1 . .
H H13A 0.5165 0.2507 0.7311 0.036 Uiso calc 1 A 1
H H13B 0.6807 0.3151 0.6884 0.036 Uiso calc 1 A 1
N N2 0.27441(16) 0.09127(13) 0.53524(11) 0.0203(3) Uani d 1 . .
C C20 0.1641(2) 0.15372(16) 0.55918(14) 0.0239(3) Uani d 1 . .
C C21 0.0256(2) 0.2359(2) 0.5910(2) 0.0417(5) Uani d 1 . .
H H21A 0.0739 0.2981 0.6665 0.063 Uiso calc 1 . .
H H21B -0.0748 0.1656 0.5921 0.063 Uiso calc 1 . .
H H21C -0.0160 0.2995 0.5360 0.063 Uiso calc 1 . .
N N3 0.43478(16) -0.20076(13) 0.54904(10) 0.0192(2) Uani d 1 . .
C C30 0.4175(2) -0.30187(16) 0.58893(12) 0.0196(3) Uani d 1 . .
C C31 0.3969(3) -0.42980(18) 0.64161(14) 0.0307(4) Uani d 1 . .
H H31A 0.4514 -0.4016 0.7234 0.046 Uiso calc 0.59(2) . .
H H31B 0.4561 -0.5108 0.6093 0.046 Uiso calc 0.59(2) . .
H H31C 0.2695 -0.4633 0.6278 0.046 Uiso calc 0.59(2) . .
H H31D 0.3332 -0.5156 0.5836 0.046 Uiso calc 0.41(2) . .
H H31E 0.3286 -0.4063 0.6977 0.046 Uiso calc 0.41(2) . .
H H31F 0.5152 -0.4539 0.6792 0.046 Uiso calc 0.41(2) . .
Co Co2 0.03936(3) 0.67240(2) 0.79974(2) 0.01989(6) Uani d 1 . .
Cl Cl3 0.20716(5) 0.50053(4) 0.86682(3) 0.02761(9) Uani d 1 . .
Cl Cl4 -0.14454(6) 0.58426(5) 0.62702(3) 0.03506(11) Uani d 1 . .
Cl Cl5A 0.2084(6) 0.8824(4) 0.7961(4) 0.0336(5) Uani d 0.76(4) B 1
Cl Cl5B 0.2143(16) 0.8801(13) 0.824(3) 0.044(3) Uani d 0.24(4) B 2
N N4 -0.13533(18) 0.71888(15) 0.89436(11) 0.0244(3) Uani d 1 . .
C C40 -0.2445(2) 0.74139(16) 0.93900(12) 0.0208(3) Uani d 1 . .
C C41 -0.3854(2) 0.77318(19) 0.99456(15) 0.0279(3) Uani d 1 . .
H H41A -0.3387 0.8522 1.0616 0.042 Uiso calc 1 . .
H H41B -0.4277 0.6828 1.0175 0.042 Uiso calc 1 . .
H H41C -0.4848 0.8060 0.9421 0.042 Uiso calc 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 0.0000 0.0000 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Co1 O1 2_656 . 180.0
O1 Co1 N3 2_656 . 89.76(4)
O1 Co1 N3 . . 90.24(4)
O1 Co1 N3 2_656 2_656 90.24(4)
O1 Co1 N3 . 2_656 89.76(4)
N3 Co1 N3 . 2_656 180.0
O1 Co1 N2 2_656 2_656 89.93(4)
O1 Co1 N2 . 2_656 90.07(4)
N3 Co1 N2 . 2_656 87.31(5)
N3 Co1 N2 2_656 2_656 92.69(5)
O1 Co1 N2 2_656 . 90.07(4)
O1 Co1 N2 . . 89.93(4)
N3 Co1 N2 . . 92.69(5)
N3 Co1 N2 2_656 . 87.31(5)
N2 Co1 N2 2_656 . 180.0
C10B O1 C13 . . 108.52(12)
C10A O1 C13 . . 108.52(12)
C10B O1 Co1 . . 124.46(9)
C10A O1 Co1 . . 124.46(9)
C13 O1 Co1 . . 124.67(9)
C11A C10A O1 . . 109.1(3)
C11A C10A H10A . . 109.9
O1 C10A H10A . . 109.9
C11A C10A H10B . . 109.9
O1 C10A H10B . . 109.9
H10A C10A H10B . . 108.3
C10A C11A C12A . . 106.4(4)
C10A C11A H11A . . 110.5
C12A C11A H11A . . 110.5
C10A C11A H11B . . 110.5
C12A C11A H11B . . 110.5
H11A C11A H11B . . 108.6
C13 C12A C11A . . 104.0(3)
C13 C12A H12A . . 111.0
C11A C12A H12A . . 111.0
C13 C12A H12B . . 111.0
C11A C12A H12B . . 111.0
H12A C12A H12B . . 109.0
O1 C10B C11B . . 105.1(2)
O1 C10B H10C . . 110.7
C11B C10B H10C . . 110.7
O1 C10B H10D . . 110.7
C11B C10B H10D . . 110.7
H10C C10B H10D . . 108.8
C12B C11B C10B . . 105.1(3)
C12B C11B H11C . . 110.7
C10B C11B H11C . . 110.7
C12B C11B H11D . . 110.7
C10B C11B H11D . . 110.7
H11C C11B H11D . . 108.8
C11B C12B C13 . . 107.7(2)
C11B C12B H12C . . 110.2
C13 C12B H12C . . 110.2
C11B C12B H12D . . 110.2
C13 C12B H12D . . 110.2
H12C C12B H12D . . 108.5
O1 C13 C12B . . 106.13(13)
O1 C13 C12A . . 106.13(13)
O1 C13 H13A . . 110.5
C12A C13 H13A . . 110.5
O1 C13 H13B . . 110.5
C12A C13 H13B . . 110.5
H13A C13 H13B . . 108.7
C20 N2 Co1 . . 172.92(12)
N2 C20 C21 . . 178.93(17)
C20 C21 H21A . . 109.5
C20 C21 H21B . . 109.5
H21A C21 H21B . . 109.5
C20 C21 H21C . . 109.5
H21A C21 H21C . . 109.5
H21B C21 H21C . . 109.5
C30 N3 Co1 . . 170.53(12)
N3 C30 C31 . . 179.12(17)
C30 C31 H31A . . 109.5
C30 C31 H31B . . 109.5
H31A C31 H31B . . 109.5
C30 C31 H31C . . 109.5
H31A C31 H31C . . 109.5
H31B C31 H31C . . 109.5
C30 C31 H31D . . 109.5
H31A C31 H31D . . 141.1
H31B C31 H31D . . 56.3
H31C C31 H31D . . 56.3
C30 C31 H31E . . 109.5
H31A C31 H31E . . 56.3
H31B C31 H31E . . 141.1
H31C C31 H31E . . 56.3
H31D C31 H31E . . 109.5
C30 C31 H31F . . 109.5
H31A C31 H31F . . 56.3
H31B C31 H31F . . 56.3
H31C C31 H31F . . 141.1
H31D C31 H31F . . 109.5
H31E C31 H31F . . 109.5
N4 Co2 Cl5B . . 106.1(7)
N4 Co2 Cl4 . . 102.04(4)
Cl5B Co2 Cl4 . . 118.0(9)
N4 Co2 Cl3 . . 109.16(4)
Cl5B Co2 Cl3 . . 108.4(4)
Cl4 Co2 Cl3 . . 112.505(17)
N4 Co2 Cl5A . . 111.05(9)
Cl4 Co2 Cl5A . . 109.56(14)
Cl3 Co2 Cl5A . . 112.10(13)
C40 N4 Co2 . . 174.12(13)
N4 C40 C41 . . 178.57(16)
C40 C41 H41A . . 109.5
C40 C41 H41B . . 109.5
H41A C41 H41B . . 109.5
C40 C41 H41C . . 109.5
H41A C41 H41C . . 109.5
H41B C41 H41C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O1 2_656 2.0888(10)
Co1 O1 . 2.0888(10)
Co1 N3 . 2.0979(12)
Co1 N3 2_656 2.0979(12)
Co1 N2 2_656 2.1017(12)
Co1 N2 . 2.1017(12)
O1 C10B . 1.4465(19)
O1 C10A . 1.4465(19)
O1 C13 . 1.4591(17)
C10A C11A . 1.425(8)
C10A H10A . 0.9900
C10A H10B . 0.9900
C11A C12A . 1.523(7)
C11A H11A . 0.9900
C11A H11B . 0.9900
C12A C13 . 1.494(2)
C12A H12A . 0.9900
C12A H12B . 0.9900
C10B C11B . 1.507(5)
C10B H10C . 0.9900
C10B H10D . 0.9900
C11B C12B . 1.466(5)
C11B H11C . 0.9900
C11B H11D . 0.9900
C12B C13 . 1.494(2)
C12B H12C . 0.9900
C12B H12D . 0.9900
C13 H13A . 0.9900
C13 H13B . 0.9900
N2 C20 . 1.1334(19)
C20 C21 . 1.449(2)
C21 H21A . 0.9800
C21 H21B . 0.9800
C21 H21C . 0.9800
N3 C30 . 1.1354(19)
C30 C31 . 1.451(2)
C31 H31A . 0.9800
C31 H31B . 0.9800
C31 H31C . 0.9800
C31 H31D . 0.9800
C31 H31E . 0.9800
C31 H31F . 0.9800
Co2 N4 . 2.0248(13)
Co2 Cl5B . 2.190(13)
Co2 Cl4 . 2.2439(5)
Co2 Cl3 . 2.2479(4)
Co2 Cl5A . 2.264(4)
N4 C40 . 1.134(2)
C40 C41 . 1.451(2)
C41 H41A . 0.9800
C41 H41B . 0.9800
C41 H41C . 0.9800
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
C13 O1 C10A C11A 0.8(5)
Co1 O1 C10A C11A -162.5(5)
O1 C10A C11A C12A -15.4(8)
C10A C11A C12A C13 23.6(7)
C13 O1 C10B C11B -25.8(4)
Co1 O1 C10B C11B 171.0(4)
O1 C10B C11B C12B 27.1(6)
C10B C11B C12B C13 -18.5(6)
C10B O1 C13 C12B 14.4(2)
Co1 O1 C13 C12B 177.62(10)
C10A O1 C13 C12A 14.4(2)
Co1 O1 C13 C12A 177.62(10)
C11B C12B C13 O1 3.1(4)
C11A C12A C13 O1 -22.9(5)

_cod_database_fobs_code 2020726
