#------------------------------------------------------------------------------
#$Date: 2017-07-25 11:46:04 +0300 (Tue, 25 Jul 2017) $
#$Revision: 199049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/80/2108081.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_2108081
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                   20.334(5)
_cell_length_b                   20.334(5)
_cell_length_c                   8.945(5)
_cell_measurement_reflns_used    26508
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.6
_cell_measurement_theta_min      0.91
_cell_volume                     3203(2)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.1423
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            26508
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.619
_diffrn_reflns_theta_min         0.912
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS, 2008'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.237
_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         0.511
_refine_diff_density_min         -0.684
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.0930
_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)+(0.1318P)²+4.8693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2479
_refine_ls_wR_factor_ref         0.2730
_reflns_number_gt                2591
_reflns_number_total             4414
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ps5056sup1.cif
_cod_data_source_block           2S_200K
_cod_database_code               2108081
_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   0.938
_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
Co Co1 0.5000 0.0000 1.0000 0.0268(3) Uani d 1
Cl Cl2 0.26017(14) -0.27676(13) 1.2307(3) 0.0805(7) Uani d 1
Cl Cl1 0.29372(14) -0.24450(16) 0.6341(3) 0.0896(9) Uani d 1
O O2 0.4545(2) 0.0113(2) 1.1891(4) 0.0326(9) Uani d 1
O O1 0.4434(2) 0.0477(2) 0.9122(4) 0.0345(10) Uani d 1
N N1 0.4064(3) -0.1120(3) 0.9720(6) 0.0375(12) Uani d 1
C C2 0.4176(3) 0.0477(3) 1.1675(6) 0.0325(13) Uani d 1
C C3 0.3832(3) 0.0684(3) 1.2851(6) 0.0312(13) Uani d 1
C C7 0.3884(4) 0.0464(4) 1.4475(7) 0.0398(15) Uani d 1
C C4 0.3458(4) 0.1049(3) 1.2447(7) 0.0362(14) Uani d 1
H H4 0.3216 0.1178 1.3210 0.043 Uiso calc 1
C C11 0.2938(4) 0.1650(4) 1.0619(8) 0.0418(15) Uani d 1
C C5 0.3401(4) 0.1257(3) 1.0926(7) 0.0370(14) Uani d 1
C C1 0.4125(3) 0.0678(3) 1.0137(6) 0.0278(12) Uani d 1
C C6 0.3744(3) 0.1085(3) 0.9824(7) 0.0334(13) Uani d 1
H H6 0.3728 0.1238 0.8827 0.040 Uiso calc 1
C C18 0.3206(4) -0.2123(5) 0.8171(9) 0.0539(19) Uani d 1
C C19 0.3824(4) -0.1404(4) 0.8373(7) 0.0445(16) Uani d 1
H H19 0.4083 -0.1107 0.7522 0.053 Uiso calc 1
C C8 0.4702(4) 0.0803(4) 1.4955(7) 0.0478(17) Uani d 1
H H8A 0.4971 0.1352 1.4774 0.072 Uiso calc 1
H H8B 0.4943 0.0571 1.4380 0.072 Uiso calc 1
H H8C 0.4722 0.0707 1.6022 0.072 Uiso calc 1
C C16 0.3068(4) -0.2261(4) 1.0735(8) 0.0493(17) Uani d 1
C C17 0.2817(4) -0.2563(4) 0.9341(10) 0.059(2) Uani d 1
H H17 0.2390 -0.3056 0.9208 0.070 Uiso calc 1
C C13 0.3026(6) 0.1939(6) 0.9046(10) 0.085(3) Uani d 1
H H13A 0.2867 0.2320 0.8993 0.127 Uiso calc 1
H H13B 0.2710 0.1516 0.8375 0.127 Uiso calc 1
H H13C 0.3560 0.2169 0.8744 0.127 Uiso calc 1
C C15 0.3696(4) -0.1544(4) 1.0898(8) 0.0452(16) Uani d 1
H H15 0.3867 -0.1350 1.1875 0.054 Uiso calc 1
C C9 0.3472(5) -0.0400(4) 1.4628(8) 0.0536(19) Uani d 1
H H9A 0.3747 -0.0601 1.4064 0.080 Uiso calc 1
H H9B 0.2955 -0.0618 1.4233 0.080 Uiso calc 1
H H9C 0.3450 -0.0537 1.5685 0.080 Uiso calc 1
C C10 0.3491(5) 0.0749(5) 1.5553(8) 0.060(2) Uani d 1
H H10A 0.3490 0.0563 1.6564 0.090 Uiso calc 1
H H10B 0.2966 0.0560 1.5225 0.090 Uiso calc 1
H H10C 0.3765 0.1306 1.5556 0.090 Uiso calc 1
C C14 0.3197(5) 0.2346(5) 1.1643(10) 0.067(2) Uani d 1
H H14A 0.3216 0.2200 1.2681 0.101 Uiso calc 1
H H14B 0.2838 0.2532 1.1565 0.101 Uiso calc 1
H H14C 0.3703 0.2747 1.1337 0.101 Uiso calc 1
C C12 0.2116(4) 0.1095(5) 1.0933(12) 0.078(3) Uani d 1
H H12A 0.2071 0.0844 1.1893 0.117 Uiso calc 1
H H12B 0.1910 0.0713 1.0136 0.117 Uiso calc 1
H H12C 0.1831 0.1366 1.0973 0.117 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 0.0015 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'
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'
O O 0.0056 0.0036 '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
O2 Co1 O2 4_657 . 180.0
O2 Co1 O1 4_657 4_657 82.24(15)
O2 Co1 O1 . 4_657 97.76(15)
O2 Co1 O1 4_657 . 97.76(15)
O2 Co1 O1 . . 82.24(15)
O1 Co1 O1 4_657 . 180.0
O2 Co1 N1 4_657 . 89.70(18)
O2 Co1 N1 . . 90.30(18)
O1 Co1 N1 4_657 . 87.17(17)
O1 Co1 N1 . . 92.83(17)
O2 Co1 N1 4_657 4_657 90.30(18)
O2 Co1 N1 . 4_657 89.70(18)
O1 Co1 N1 4_657 4_657 92.83(17)
O1 Co1 N1 . 4_657 87.17(17)
N1 Co1 N1 . 4_657 180.0
C2 O2 Co1 . . 111.8(3)
C1 O1 Co1 . . 111.7(3)
C19 N1 C15 . . 118.3(6)
C19 N1 Co1 . . 120.8(5)
C15 N1 Co1 . . 120.9(5)
O2 C2 C3 . . 124.0(5)
O2 C2 C1 . . 116.2(5)
C3 C2 C1 . . 119.7(5)
C4 C3 C2 . . 117.1(5)
C4 C3 C7 . . 123.5(5)
C2 C3 C7 . . 119.4(5)
C8 C7 C9 . . 110.1(6)
C8 C7 C3 . . 110.9(5)
C9 C7 C3 . . 109.9(5)
C8 C7 C10 . . 108.1(6)
C9 C7 C10 . . 106.7(6)
C3 C7 C10 . . 111.0(5)
C3 C4 C5 . . 124.1(6)
C13 C11 C12 . . 109.9(7)
C13 C11 C5 . . 112.8(6)
C12 C11 C5 . . 108.6(6)
C13 C11 C14 . . 106.2(7)
C12 C11 C14 . . 108.7(7)
C5 C11 C14 . . 110.7(5)
C6 C5 C4 . . 119.0(5)
C6 C5 C11 . . 122.3(6)
C4 C5 C11 . . 118.6(6)
O1 C1 C6 . . 123.0(5)
O1 C1 C2 . . 117.7(5)
C6 C1 C2 . . 119.3(5)
C5 C6 C1 . . 120.7(6)
C17 C18 C19 . . 121.5(7)
C17 C18 Cl1 . . 120.7(6)
C19 C18 Cl1 . . 117.8(6)
N1 C19 C18 . . 121.6(7)
C17 C16 C15 . . 120.6(7)
C17 C16 Cl2 . . 120.3(6)
C15 C16 Cl2 . . 119.1(6)
C18 C17 C16 . . 116.5(7)
N1 C15 C16 . . 121.6(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O2 4_657 1.995(4)
Co1 O2 . 1.995(4)
Co1 O1 4_657 2.000(4)
Co1 O1 . 2.000(4)
Co1 N1 . 2.130(5)
Co1 N1 4_657 2.130(5)
Cl2 C16 . 1.720(8)
Cl1 C18 . 1.746(8)
O2 C2 . 1.305(7)
O1 C1 . 1.282(7)
N1 C19 . 1.320(8)
N1 C15 . 1.330(8)
C2 C3 . 1.439(8)
C2 C1 . 1.454(8)
C3 C4 . 1.351(8)
C3 C7 . 1.539(8)
C7 C8 . 1.509(10)
C7 C9 . 1.530(9)
C7 C10 . 1.539(9)
C4 C5 . 1.446(9)
C11 C13 . 1.501(10)
C11 C12 . 1.503(10)
C11 C5 . 1.534(8)
C11 C14 . 1.541(10)
C5 C6 . 1.350(9)
C1 C6 . 1.416(8)
C18 C17 . 1.347(11)
C18 C19 . 1.384(10)
C16 C17 . 1.371(11)
C16 C15 . 1.383(10)
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
Co1 O2 C2 C3 -175.8(5)
Co1 O2 C2 C1 3.8(6)
O2 C2 C3 C4 -178.9(6)
C1 C2 C3 C4 1.4(8)
O2 C2 C3 C7 -0.7(9)
C1 C2 C3 C7 179.6(5)
C4 C3 C7 C8 -122.9(6)
C2 C3 C7 C8 59.0(7)
C4 C3 C7 C9 115.1(7)
C2 C3 C7 C9 -63.0(7)
C4 C3 C7 C10 -2.7(9)
C2 C3 C7 C10 179.2(6)
C2 C3 C4 C5 -1.6(9)
C7 C3 C4 C5 -179.7(6)
C3 C4 C5 C6 -0.4(10)
C3 C4 C5 C11 178.2(6)
C13 C11 C5 C6 -10.3(10)
C12 C11 C5 C6 111.6(8)
C14 C11 C5 C6 -129.1(7)
C13 C11 C5 C4 171.1(7)
C12 C11 C5 C4 -66.9(8)
C14 C11 C5 C4 52.3(8)
Co1 O1 C1 C6 174.7(4)
Co1 O1 C1 C2 -5.2(6)
O2 C2 C1 O1 0.9(8)
C3 C2 C1 O1 -179.4(5)
O2 C2 C1 C6 -179.0(5)
C3 C2 C1 C6 0.7(8)
C4 C5 C6 C1 2.7(9)
C11 C5 C6 C1 -175.9(5)
O1 C1 C6 C5 177.3(6)
C2 C1 C6 C5 -2.8(8)
C15 N1 C19 C18 0.0(9)
Co1 N1 C19 C18 -178.4(5)
C17 C18 C19 N1 0.6(11)
Cl1 C18 C19 N1 -179.8(5)
C19 C18 C17 C16 -0.3(11)
Cl1 C18 C17 C16 -179.8(5)
C15 C16 C17 C18 -0.7(11)
Cl2 C16 C17 C18 178.8(6)
C19 N1 C15 C16 -1.0(9)
Co1 N1 C15 C16 177.4(5)
C17 C16 C15 N1 1.4(11)
Cl2 C16 C15 N1 -178.1(5)
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 -0.049 435 163 ' '

_cod_database_fobs_code 2108081
