#------------------------------------------------------------------------------
#$Date: 2017-07-25 11:46:04 +0300 (Tue, 25 Jul 2017) $
#$Revision: 199049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/80/2108075.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_2108075
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 Br4 Co N2 O4'
_chemical_formula_weight         973.34
_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
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.3624(10)
_cell_length_b                   20.3624(10)
_cell_length_c                   9.0045(5)
_cell_measurement_reflns_used    33637
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      23.66
_cell_measurement_theta_min      0.91
_cell_volume                     3233.3(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      175(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_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  0.0920
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            33637
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.663
_diffrn_reflns_theta_min         0.911
_exptl_absorpt_coefficient_mu    2.215
_exptl_absorpt_correction_T_max  0.718
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS, 2008'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             1461
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_platon_squeeze_details
;
;
_refine_diff_density_max         0.717
_refine_diff_density_min         -1.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         6344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.0726
_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)+(0.0893P)²+4.9086P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2044
_reflns_number_gt                3377
_reflns_number_total             6344
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ps5056sup1.cif
_cod_data_source_block           1S_175K
_cod_original_cell_volume        3233.3(4)
_cod_database_code               2108075
_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   0.607
_shelx_estimated_absorpt_t_max   0.718
_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 0.4121(3) 0.0665(3) 0.9844(6) 0.0202(10) Uani d 1
C C2 0.4174(3) 0.0466(3) 0.8331(6) 0.0201(11) Uani d 1
C C3 0.3833(3) 0.0671(3) 0.7169(6) 0.0243(11) Uani d 1
C C4 0.3456(3) 0.1045(3) 0.7573(7) 0.0271(12) Uani d 1
H H4 0.3222 0.1177 0.6809 0.033 Uiso calc 1
C C5 0.3393(3) 0.1247(3) 0.9058(6) 0.0256(12) Uani d 1
C C6 0.3726(3) 0.1061(3) 1.0183(6) 0.0239(11) Uani d 1
H H6 0.3693 0.1195 1.1180 0.029 Uiso calc 1
C C7 0.3874(3) 0.0449(3) 0.5552(6) 0.0287(12) Uani d 1
C C8 0.4709(3) 0.0786(4) 0.5044(7) 0.0365(14) Uani d 1
H H8A 0.4977 0.1338 0.5166 0.055 Uiso calc 1
H H8B 0.4721 0.0662 0.3996 0.055 Uiso calc 1
H H8C 0.4956 0.0572 0.5647 0.055 Uiso calc 1
C C9 0.3460(4) -0.0423(3) 0.5409(7) 0.0379(15) Uani d 1
H H9A 0.3699 -0.0626 0.6069 0.057 Uiso calc 1
H H9B 0.3492 -0.0561 0.4380 0.057 Uiso calc 1
H H9C 0.2926 -0.0636 0.5687 0.057 Uiso calc 1
C C10 0.3492(4) 0.0749(4) 0.4492(7) 0.0448(17) Uani d 1
H H10A 0.2968 0.0564 0.4812 0.067 Uiso calc 1
H H10B 0.3493 0.0570 0.3482 0.067 Uiso calc 1
H H10C 0.3772 0.1305 0.4506 0.067 Uiso calc 1
C C11 0.2939(3) 0.1642(3) 0.9381(7) 0.0294(13) Uani d 1
C C12 0.3205(4) 0.2327(4) 0.8379(9) 0.052(2) Uani d 1
H H12A 0.2904 0.2572 0.8577 0.079 Uiso calc 1
H H12B 0.3140 0.2165 0.7338 0.079 Uiso calc 1
H H12C 0.3741 0.2687 0.8572 0.079 Uiso calc 1
C C13 0.2972(6) 0.1873(6) 1.0954(9) 0.071(3) Uani d 1
H H13A 0.3503 0.2196 1.1251 0.106 Uiso calc 1
H H13B 0.2734 0.1421 1.1586 0.106 Uiso calc 1
H H13C 0.2702 0.2156 1.1065 0.106 Uiso calc 1
C C14 0.2102(4) 0.1084(4) 0.8959(12) 0.068(3) Uani d 1
H H14A 0.1901 0.0635 0.9601 0.103 Uiso calc 1
H H14B 0.2076 0.0929 0.7920 0.103 Uiso calc 1
H H14C 0.1801 0.1333 0.9089 0.103 Uiso calc 1
C C15 0.3684(3) -0.1538(3) 0.9163(7) 0.0326(13) Uani d 1
H H15 0.3839 -0.1359 0.8179 0.039 Uiso calc 1
C C16 0.3054(3) -0.2257(3) 0.9381(7) 0.0317(13) Uani d 1
C C17 0.2819(4) -0.2536(4) 1.0797(7) 0.0365(14) Uani d 1
H H17 0.2384 -0.3020 1.0959 0.044 Uiso calc 1
C C18 0.3235(3) -0.2089(4) 1.1953(7) 0.0359(14) Uani d 1
C C19 0.3846(3) -0.1379(4) 1.1696(7) 0.0352(14) Uani d 1
H H19 0.4119 -0.1072 1.2520 0.042 Uiso calc 1
N N1 0.4071(3) -0.1101(3) 1.0298(5) 0.0274(10) Uani d 1
O O1 0.4436(2) 0.0466(2) 1.0880(4) 0.0250(8) Uani d 1
O O2 0.4541(2) 0.01003(19) 0.8117(4) 0.0237(8) Uani d 1
Co Co1 0.5000 0.0000 1.0000 0.0185(2) Uani d 1
Br Br1 0.29720(4) -0.23959(4) 1.39293(8) 0.0550(3) Uani d 1
Br Br2 0.25137(4) -0.28270(4) 0.77087(8) 0.0496(2) 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'
Co Co 0.3050 0.6296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.1811 1.6452 '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 . . 121.6(5)
O1 C1 C2 . . 118.1(4)
C6 C1 C2 . . 120.2(5)
O2 C2 C3 . . 124.0(5)
O2 C2 C1 . . 116.4(5)
C3 C2 C1 . . 119.6(4)
C4 C3 C2 . . 117.2(5)
C4 C3 C7 . . 122.7(5)
C2 C3 C7 . . 120.1(5)
C3 C4 C5 . . 124.5(5)
C3 C4 H4 . . 117.8
C5 C4 H4 . . 117.8
C6 C5 C4 . . 119.0(5)
C6 C5 C11 . . 121.1(5)
C4 C5 C11 . . 119.9(5)
C5 C6 C1 . . 119.5(5)
C5 C6 H6 . . 120.2
C1 C6 H6 . . 120.2
C10 C7 C3 . . 111.1(5)
C10 C7 C9 . . 108.2(5)
C3 C7 C9 . . 109.8(5)
C10 C7 C8 . . 107.5(5)
C3 C7 C8 . . 110.9(5)
C9 C7 C8 . . 109.3(5)
C7 C8 H8A . . 109.5
C7 C8 H8B . . 109.5
H8A C8 H8B . . 109.5
C7 C8 H8C . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
C7 C9 H9A . . 109.5
C7 C9 H9B . . 109.5
H9A C9 H9B . . 109.5
C7 C9 H9C . . 109.5
H9A C9 H9C . . 109.5
H9B C9 H9C . . 109.5
C7 C10 H10A . . 109.5
C7 C10 H10B . . 109.5
H10A C10 H10B . . 109.5
C7 C10 H10C . . 109.5
H10A C10 H10C . . 109.5
H10B C10 H10C . . 109.5
C13 C11 C12 . . 109.8(6)
C13 C11 C5 . . 113.9(5)
C12 C11 C5 . . 109.8(5)
C13 C11 C14 . . 109.1(6)
C12 C11 C14 . . 106.6(6)
C5 C11 C14 . . 107.4(5)
C11 C12 H12A . . 109.5
C11 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
C11 C12 H12C . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
C11 C13 H13A . . 109.5
C11 C13 H13B . . 109.5
H13A C13 H13B . . 109.5
C11 C13 H13C . . 109.5
H13A C13 H13C . . 109.5
H13B C13 H13C . . 109.5
C11 C14 H14A . . 109.5
C11 C14 H14B . . 109.5
H14A C14 H14B . . 109.5
C11 C14 H14C . . 109.5
H14A C14 H14C . . 109.5
H14B C14 H14C . . 109.5
N1 C15 C16 . . 121.4(6)
N1 C15 H15 . . 119.3
C16 C15 H15 . . 119.3
C17 C16 C15 . . 120.6(6)
C17 C16 Br2 . . 120.6(5)
C15 C16 Br2 . . 118.7(5)
C18 C17 C16 . . 117.3(6)
C18 C17 H17 . . 121.3
C16 C17 H17 . . 121.3
C17 C18 C19 . . 120.4(6)
C17 C18 Br1 . . 121.6(5)
C19 C18 Br1 . . 117.9(5)
N1 C19 C18 . . 122.1(6)
N1 C19 H19 . . 118.9
C18 C19 H19 . . 118.9
C15 N1 C19 . . 118.0(5)
C15 N1 Co1 . . 122.2(4)
C19 N1 Co1 . . 119.8(4)
C1 O1 Co1 . . 110.7(3)
C2 O2 Co1 . . 111.4(3)
O1 Co1 O1 4_657 . 180.0
O1 Co1 O2 4_657 . 97.05(14)
O1 Co1 O2 . . 82.95(14)
O1 Co1 O2 4_657 4_657 82.95(14)
O1 Co1 O2 . 4_657 97.05(14)
O2 Co1 O2 . 4_657 180.0
O1 Co1 N1 4_657 . 88.20(16)
O1 Co1 N1 . . 91.80(16)
O2 Co1 N1 . . 89.98(16)
O2 Co1 N1 4_657 . 90.02(16)
O1 Co1 N1 4_657 4_657 91.80(16)
O1 Co1 N1 . 4_657 88.20(16)
O2 Co1 N1 . 4_657 90.02(16)
O2 Co1 N1 4_657 4_657 89.98(16)
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 . 1.305(6)
C1 C6 . 1.430(7)
C1 C2 . 1.440(7)
C2 O2 . 1.305(6)
C2 C3 . 1.429(7)
C3 C4 . 1.372(7)
C3 C7 . 1.538(8)
C4 C5 . 1.424(8)
C4 H4 . 0.9500
C5 C6 . 1.373(8)
C5 C11 . 1.527(7)
C6 H6 . 0.9500
C7 C10 . 1.537(8)
C7 C9 . 1.544(8)
C7 C8 . 1.551(8)
C8 H8A . 0.9800
C8 H8B . 0.9800
C8 H8C . 0.9800
C9 H9A . 0.9800
C9 H9B . 0.9800
C9 H9C . 0.9800
C10 H10A . 0.9800
C10 H10B . 0.9800
C10 H10C . 0.9800
C11 C13 . 1.483(10)
C11 C12 . 1.516(9)
C11 C14 . 1.550(10)
C12 H12A . 0.9800
C12 H12B . 0.9800
C12 H12C . 0.9800
C13 H13A . 0.9800
C13 H13B . 0.9800
C13 H13C . 0.9800
C14 H14A . 0.9800
C14 H14B . 0.9800
C14 H14C . 0.9800
C15 N1 . 1.326(8)
C15 C16 . 1.397(8)
C15 H15 . 0.9500
C16 C17 . 1.380(9)
C16 Br2 . 1.883(6)
C17 C18 . 1.363(9)
C17 H17 . 0.9500
C18 C19 . 1.376(9)
C18 Br1 . 1.873(6)
C19 N1 . 1.363(8)
C19 H19 . 0.9500
N1 Co1 . 2.106(5)
O1 Co1 . 1.985(4)
O2 Co1 . 1.995(4)
Co1 O1 4_657 1.985(4)
Co1 O2 4_657 1.995(4)
Co1 N1 4_657 2.106(5)
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 -0.4(6)
C6 C1 C2 O2 -179.6(4)
O1 C1 C2 C3 179.7(4)
C6 C1 C2 C3 0.5(7)
O2 C2 C3 C4 179.0(5)
C1 C2 C3 C4 -1.1(7)
O2 C2 C3 C7 1.1(8)
C1 C2 C3 C7 -178.9(4)
C2 C3 C4 C5 0.9(8)
C7 C3 C4 C5 178.7(5)
C3 C4 C5 C6 -0.1(8)
C3 C4 C5 C11 -178.2(5)
C4 C5 C6 C1 -0.5(8)
C11 C5 C6 C1 177.5(5)
O1 C1 C6 C5 -178.9(5)
C2 C1 C6 C5 0.3(7)
C4 C3 C7 C10 4.0(8)
C2 C3 C7 C10 -178.3(5)
C4 C3 C7 C9 -115.6(6)
C2 C3 C7 C9 62.1(7)
C4 C3 C7 C8 123.5(6)
C2 C3 C7 C8 -58.8(6)
C6 C5 C11 C13 6.6(9)
C4 C5 C11 C13 -175.4(6)
C6 C5 C11 C12 130.2(6)
C4 C5 C11 C12 -51.8(7)
C6 C5 C11 C14 -114.3(7)
C4 C5 C11 C14 63.7(7)
N1 C15 C16 C17 -0.5(8)
N1 C15 C16 Br2 177.7(4)
C15 C16 C17 C18 -1.4(8)
Br2 C16 C17 C18 -179.5(4)
C16 C17 C18 C19 2.4(9)
C16 C17 C18 Br1 179.4(4)
C17 C18 C19 N1 -1.7(9)
Br1 C18 C19 N1 -178.8(4)
C16 C15 N1 C19 1.3(8)
C16 C15 N1 Co1 -177.8(4)
C18 C19 N1 C15 -0.3(8)
C18 C19 N1 Co1 178.9(4)
C6 C1 O1 Co1 -175.6(4)
C2 C1 O1 Co1 5.1(5)
C3 C2 O2 Co1 175.3(4)
C1 C2 O2 Co1 -4.6(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 -0.049 438 192 ' '

_cod_database_fobs_code 2108075
