#------------------------------------------------------------------------------
#$Date: 2017-07-25 11:46:04 +0300 (Tue, 25 Jul 2017) $
#$Revision: 199049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/80/2108080.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_2108080
loop_
_publ_author_name
'Hathwar, Venkatesha R.'
'Stingaciu, Marian'
'Richter, Bo'
'Overgaard, Jacob'
'Iversen, Bo B.'
_publ_section_title
;
 Variable-temperature structural studies on valence tautomerism in cobalt
 bis(dioxolene) molecular complexes
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              304
_journal_page_last               312
_journal_paper_doi               10.1107/S2052520616019235
_journal_volume                  73
_journal_year                    2017
_chemical_formula_sum            'C38 H46 Cl4 Co N2 O4'
_chemical_formula_weight         795.50
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                120.000(5)
_cell_formula_units_Z            3
_cell_length_a                   20.243(5)
_cell_length_b                   20.243(5)
_cell_length_c                   8.933(5)
_cell_measurement_reflns_used    13452
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      20.55
_cell_measurement_theta_min      0.92
_cell_volume                     3170(2)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      175(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.1296
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13452
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.552
_diffrn_reflns_theta_min         0.917
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS, 2008'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             1245
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.499
_refine_ls_extinction_coef       0.022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1692
_refine_ls_R_factor_gt           0.1051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1396P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2779
_refine_ls_wR_factor_ref         0.3073
_reflns_number_gt                2085
_reflns_number_total             4286
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ps5056sup1.cif
_cod_data_source_block           2S_175K
_cod_database_code               2108080
_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   0.937
_shelx_estimated_absorpt_t_max   0.965
_shelxl_version_number           201.4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
C C1 0.6544(4) 0.0678(4) 0.9859(7) 0.0284(15) Uani d 1
C C2 0.6286(4) 0.0476(4) 0.8355(7) 0.0303(16) Uani d 1
C C3 0.6848(4) 0.0684(4) 0.7170(8) 0.0370(18) Uani d 1
C C4 0.7599(4) 0.1061(4) 0.7575(8) 0.0369(17) Uani d 1
H H4 0.7972 0.1192 0.6813 0.044 Uiso calc 1
C C5 0.7855(4) 0.1270(4) 0.9091(8) 0.0375(18) Uani d 1
C C6 0.7339(4) 0.1087(4) 1.0185(8) 0.0380(18) Uani d 1
H H6 0.7505 0.1232 1.1187 0.046 Uiso calc 1
C C7 0.6571(4) 0.0464(4) 0.5532(8) 0.0415(19) Uani d 1
C C8 0.6115(5) -0.0402(5) 0.5373(10) 0.054(2) Uani d 1
H H8A 0.6412 -0.0623 0.5775 0.080 Uiso calc 1
H H8B 0.6004 -0.0537 0.4313 0.080 Uiso calc 1
H H8C 0.5635 -0.0602 0.5929 0.080 Uiso calc 1
C C9 0.6083(5) 0.0797(5) 0.5041(9) 0.046(2) Uani d 1
H H9A 0.5600 0.0550 0.5593 0.069 Uiso calc 1
H H9B 0.5981 0.0712 0.3966 0.069 Uiso calc 1
H H9C 0.6353 0.1347 0.5247 0.069 Uiso calc 1
C C10 0.7260(5) 0.0748(5) 0.4484(9) 0.055(2) Uani d 1
H H10A 0.7584 0.1302 0.4587 0.083 Uiso calc 1
H H10B 0.7083 0.0622 0.3447 0.083 Uiso calc 1
H H10C 0.7555 0.0500 0.4749 0.083 Uiso calc 1
C C11 0.8716(4) 0.1655(4) 0.9411(9) 0.0426(19) Uani d 1
C C12 0.8968(6) 0.1086(6) 0.9115(15) 0.088(4) Uani d 1
H H12A 0.9438 0.1326 0.8521 0.132 Uiso calc 1
H H12B 0.8568 0.0651 0.8561 0.132 Uiso calc 1
H H12C 0.9062 0.0907 1.0068 0.132 Uiso calc 1
C C13 0.8910(6) 0.1960(8) 1.0951(13) 0.104(5) Uani d 1
H H13A 0.9426 0.2405 1.0964 0.156 Uiso calc 1
H H13B 0.8889 0.1566 1.1620 0.156 Uiso calc 1
H H13C 0.8545 0.2112 1.1290 0.156 Uiso calc 1
C C14 0.9150(5) 0.2339(6) 0.8340(11) 0.069(3) Uani d 1
H H14A 0.9047 0.2748 0.8619 0.104 Uiso calc 1
H H14B 0.8980 0.2177 0.7310 0.104 Uiso calc 1
H H14C 0.9699 0.2528 0.8414 0.104 Uiso calc 1
C C15 0.4745(4) -0.1525(5) 0.9083(10) 0.052(2) Uani d 1
H H15 0.4747 -0.1340 0.8105 0.063 Uiso calc 1
C C16 0.4663(5) -0.2244(5) 0.9261(10) 0.049(2) Uani d 1
C C17 0.4623(5) -0.2543(5) 1.0674(11) 0.056(2) Uani d 1
H H17 0.4555 -0.3039 1.0809 0.067 Uiso calc 1
C C18 0.4684(5) -0.2102(5) 1.1841(10) 0.053(2) Uani d 1
C C19 0.4789(5) -0.1363(5) 1.1623(10) 0.052(2) Uani d 1
H H19 0.4836 -0.1057 1.2466 0.062 Uiso calc 1
N N1 0.4822(3) -0.1094(4) 1.0259(7) 0.0406(16) Uani d 1
O O1 0.6016(3) 0.0467(3) 1.0898(5) 0.0377(12) Uani d 1
O O2 0.5547(3) 0.0111(3) 0.8133(5) 0.0340(12) Uani d 1
Cl Cl1 0.46394(18) -0.24181(18) 1.3656(3) 0.0841(10) Uani d 1
Cl Cl2 0.46222(16) -0.27512(14) 0.7660(3) 0.0743(8) Uani d 1
Co Co1 0.5000 0.0000 1.0000 0.0279(5) Uani d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3050 0.6296 '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 C1 C6 . . 122.9(6)
O1 C1 C2 . . 116.9(6)
C6 C1 C2 . . 120.3(6)
O2 C2 C1 . . 117.0(6)
O2 C2 C3 . . 124.1(6)
C1 C2 C3 . . 118.9(6)
C4 C3 C2 . . 117.4(6)
C4 C3 C7 . . 123.6(7)
C2 C3 C7 . . 119.1(6)
C3 C4 C5 . . 123.5(7)
C6 C5 C4 . . 119.3(7)
C6 C5 C11 . . 122.3(7)
C4 C5 C11 . . 118.3(7)
C5 C6 C1 . . 120.6(7)
C9 C7 C8 . . 109.3(7)
C9 C7 C10 . . 109.3(7)
C8 C7 C10 . . 106.7(7)
C9 C7 C3 . . 111.7(6)
C8 C7 C3 . . 110.0(6)
C10 C7 C3 . . 109.7(6)
C13 C11 C12 . . 111.3(9)
C13 C11 C5 . . 112.4(7)
C12 C11 C5 . . 108.2(7)
C13 C11 C14 . . 106.8(8)
C12 C11 C14 . . 108.7(8)
C5 C11 C14 . . 109.4(6)
N1 C15 C16 . . 120.8(9)
C17 C16 C15 . . 120.8(8)
C17 C16 Cl2 . . 121.1(7)
C15 C16 Cl2 . . 118.0(7)
C18 C17 C16 . . 116.9(9)
C17 C18 C19 . . 120.9(8)
C17 C18 Cl1 . . 120.9(7)
C19 C18 Cl1 . . 118.2(7)
N1 C19 C18 . . 120.8(8)
C19 N1 C15 . . 119.6(8)
C19 N1 Co1 . . 119.3(6)
C15 N1 Co1 . . 121.1(6)
C1 O1 Co1 . . 110.8(4)
C2 O2 Co1 . . 111.0(4)
O2 Co1 O2 . 4_657 180.0
O2 Co1 O1 . 4_657 95.97(19)
O2 Co1 O1 4_657 4_657 84.02(19)
O2 Co1 O1 . . 84.03(19)
O2 Co1 O1 4_657 . 95.98(19)
O1 Co1 O1 4_657 . 180.0
O2 Co1 N1 . 4_657 89.8(2)
O2 Co1 N1 4_657 4_657 90.2(2)
O1 Co1 N1 4_657 4_657 92.8(2)
O1 Co1 N1 . 4_657 87.2(2)
O2 Co1 N1 . . 90.2(2)
O2 Co1 N1 4_657 . 89.8(2)
O1 Co1 N1 4_657 . 87.2(2)
O1 Co1 N1 . . 92.8(2)
N1 Co1 N1 4_657 . 180.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 O1 . 1.315(8)
C1 C6 . 1.424(10)
C1 C2 . 1.425(9)
C2 O2 . 1.311(8)
C2 C3 . 1.454(10)
C3 C4 . 1.364(10)
C3 C7 . 1.550(10)
C4 C5 . 1.437(10)
C5 C6 . 1.340(10)
C5 C11 . 1.540(10)
C7 C9 . 1.513(12)
C7 C8 . 1.526(11)
C7 C10 . 1.533(11)
C11 C13 . 1.478(13)
C11 C12 . 1.499(13)
C11 C14 . 1.545(11)
C15 N1 . 1.324(10)
C15 C16 . 1.389(12)
C16 C17 . 1.385(12)
C16 Cl2 . 1.738(9)
C17 C18 . 1.337(12)
C18 C19 . 1.415(12)
C18 Cl1 . 1.729(9)
C19 N1 . 1.323(10)
N1 Co1 . 2.071(7)
O1 Co1 . 1.955(5)
O2 Co1 . 1.952(5)
Co1 O2 4_657 1.952(5)
Co1 O1 4_657 1.955(5)
Co1 N1 4_657 2.071(7)
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
O1 C1 C2 O2 1.3(9)
C6 C1 C2 O2 -178.9(6)
O1 C1 C2 C3 -178.7(6)
C6 C1 C2 C3 1.0(10)
O2 C2 C3 C4 -179.7(7)
C1 C2 C3 C4 0.4(10)
O2 C2 C3 C7 -0.1(10)
C1 C2 C3 C7 179.9(6)
C2 C3 C4 C5 -1.1(11)
C7 C3 C4 C5 179.4(7)
C3 C4 C5 C6 0.3(11)
C3 C4 C5 C11 176.7(7)
C4 C5 C6 C1 1.1(11)
C11 C5 C6 C1 -175.1(6)
O1 C1 C6 C5 177.9(7)
C2 C1 C6 C5 -1.8(10)
C4 C3 C7 C9 -122.5(8)
C2 C3 C7 C9 58.0(9)
C4 C3 C7 C8 116.1(8)
C2 C3 C7 C8 -63.5(9)
C4 C3 C7 C10 -1.1(10)
C2 C3 C7 C10 179.4(7)
C6 C5 C11 C13 -13.8(12)
C4 C5 C11 C13 169.9(9)
C6 C5 C11 C12 109.5(9)
C4 C5 C11 C12 -66.8(10)
C6 C5 C11 C14 -132.3(8)
C4 C5 C11 C14 51.5(10)
N1 C15 C16 C17 3.1(13)
N1 C15 C16 Cl2 -176.3(6)
C15 C16 C17 C18 -1.4(13)
Cl2 C16 C17 C18 177.9(7)
C16 C17 C18 C19 -0.3(13)
C16 C17 C18 Cl1 179.8(6)
C17 C18 C19 N1 0.6(13)
Cl1 C18 C19 N1 -179.5(6)
C18 C19 N1 C15 1.0(11)
C18 C19 N1 Co1 -178.7(6)
C16 C15 N1 C19 -2.8(12)
C16 C15 N1 Co1 176.9(6)
C6 C1 O1 Co1 175.0(5)
C2 C1 O1 Co1 -5.3(7)
C1 C2 O2 Co1 3.4(7)
C3 C2 O2 Co1 -176.6(6)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.050 407 147 ' '

_cod_database_fobs_code 2108080
