#------------------------------------------------------------------------------
#$Date: 2017-07-25 11:46:04 +0300 (Tue, 25 Jul 2017) $
#$Revision: 199049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/80/2108073.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_2108073
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                   20.1281(7)
_cell_length_b                   20.1281(7)
_cell_length_c                   8.9942(3)
_cell_measurement_reflns_used    23579
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.62
_cell_measurement_theta_min      0.92
_cell_volume                     3155.72(19)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0852
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            23579
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.619
_diffrn_reflns_theta_min         0.922
_exptl_absorpt_coefficient_mu    2.270
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS, 2008'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.537
_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         0.933
_refine_diff_density_min         -0.982
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0657P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                3675
_reflns_number_total             6428
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ps5056sup1.cif
_cod_data_source_block           1S_100K
_cod_original_cell_volume        3155.7(2)
_cod_database_code               2108073
_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   0.601
_shelx_estimated_absorpt_t_max   0.713
_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 0.5850(2) 0.9330(2) 0.5125(5) 0.0109(8) Uani d 1
C C2 0.5798(2) 0.9528(2) 0.6631(5) 0.0125(9) Uani d 1
C C3 0.6136(2) 0.9323(2) 0.7802(5) 0.0132(9) Uani d 1
C C4 0.6511(2) 0.8928(2) 0.7379(5) 0.0158(9) Uani d 1
H H4 0.6739 0.8781 0.8140 0.019 Uiso calc 1
C C5 0.6577(2) 0.8731(2) 0.5894(5) 0.0147(9) Uani d 1
C C6 0.6232(2) 0.8925(2) 0.4788(5) 0.0155(9) Uani d 1
H H6 0.6253 0.8784 0.3789 0.019 Uiso calc 1
C C7 0.6103(2) 0.9544(3) 0.9412(5) 0.0155(9) Uani d 1
C C8 0.6524(3) 1.0425(2) 0.9559(6) 0.0198(10) Uani d 1
H H8A 0.6491 1.0564 1.0590 0.030 Uiso calc 1
H H8B 0.6284 1.0633 0.8899 0.030 Uiso calc 1
H H8C 0.7063 1.0638 0.9282 0.030 Uiso calc 1
C C9 0.5265(3) 0.9212(3) 0.9945(5) 0.0203(10) Uani d 1
H H9A 0.5262 0.9326 1.1003 0.030 Uiso calc 1
H H9B 0.4984 0.8655 0.9796 0.030 Uiso calc 1
H H9C 0.5018 0.9443 0.9373 0.030 Uiso calc 1
C C10 0.6486(3) 0.9238(3) 1.0474(6) 0.0250(11) Uani d 1
H H10A 0.7035 0.9485 1.0248 0.037 Uiso calc 1
H H10B 0.6251 0.8682 1.0349 0.037 Uiso calc 1
H H10C 0.6418 0.9353 1.1503 0.037 Uiso calc 1
C C11 0.7055(2) 0.8352(2) 0.5586(5) 0.0159(9) Uani d 1
C C12 0.6833(4) 0.7681(4) 0.6603(7) 0.0470(12) Uani d 1
H H12A 0.7211 0.7512 0.6522 0.070 Uiso calc 1
H H12B 0.6326 0.7259 0.6320 0.070 Uiso calc 1
H H12C 0.6817 0.7834 0.7631 0.070 Uiso calc 1
C C13 0.6972(4) 0.8062(4) 0.4039(7) 0.0470(12) Uani d 1
H H13A 0.7193 0.8496 0.3346 0.070 Uiso calc 1
H H13B 0.6427 0.7727 0.3811 0.070 Uiso calc 1
H H13C 0.7241 0.7771 0.3938 0.070 Uiso calc 1
C C14 0.7887(3) 0.8933(3) 0.5925(10) 0.059(2) Uani d 1
H H14A 0.7935 0.9088 0.6970 0.088 Uiso calc 1
H H14B 0.8055 0.9384 0.5288 0.088 Uiso calc 1
H H14C 0.8207 0.8702 0.5735 0.088 Uiso calc 1
C C15 0.6262(2) 1.1485(2) 0.5890(5) 0.0160(9) Uani d 1
H H15 0.6093 1.1300 0.6868 0.019 Uiso calc 1
C C16 0.6894(3) 1.2212(3) 0.5685(5) 0.0181(10) Uani d 1
C C17 0.7142(3) 1.2489(3) 0.4270(5) 0.0206(10) Uani d 1
H H17 0.7577 1.2982 0.4119 0.025 Uiso calc 1
C C18 0.6744(3) 1.2033(3) 0.3090(5) 0.0193(10) Uani d 1
C C19 0.6124(2) 1.1304(3) 0.3331(5) 0.0160(9) Uani d 1
H H19 0.5862 1.0987 0.2504 0.019 Uiso calc 1
N N1 0.5889(2) 1.10393(19) 0.4714(4) 0.0133(8) Uani d 1
O O1 0.55234(16) 0.95473(16) 0.4092(3) 0.0128(6) Uani d 1
O O2 0.54176(16) 0.99113(16) 0.6827(3) 0.0121(6) Uani d 1
Co Co1 0.5000 1.0000 0.5000 0.01082(19) Uani d 1
Br Br1 0.70184(3) 1.23597(3) 0.11131(6) 0.02748(15) Uani d 1
Br Br2 0.74304(3) 1.27900(3) 0.73577(6) 0.02633(15) 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 . . 122.9(4)
O1 C1 C2 . . 116.8(4)
C6 C1 C2 . . 120.2(4)
O2 C2 C3 . . 124.3(4)
O2 C2 C1 . . 115.3(4)
C3 C2 C1 . . 120.4(4)
C4 C3 C2 . . 115.9(4)
C4 C3 C7 . . 122.8(4)
C2 C3 C7 . . 121.3(4)
C3 C4 C5 . . 124.7(4)
C3 C4 H4 . . 117.6
C5 C4 H4 . . 117.6
C6 C5 C4 . . 118.1(4)
C6 C5 C11 . . 123.0(4)
C4 C5 C11 . . 118.8(4)
C5 C6 C1 . . 120.6(4)
C5 C6 H6 . . 119.7
C1 C6 H6 . . 119.7
C3 C7 C10 . . 111.6(4)
C3 C7 C8 . . 109.7(4)
C10 C7 C8 . . 108.0(4)
C3 C7 C9 . . 111.5(4)
C10 C7 C9 . . 106.9(4)
C8 C7 C9 . . 108.9(4)
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 . . 107.0(4)
C13 C11 C14 . . 110.8(5)
C12 C11 C14 . . 106.8(5)
C13 C11 C5 . . 113.1(4)
C12 C11 C5 . . 111.2(4)
C14 C11 C5 . . 107.9(4)
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 . . 120.6(4)
N1 C15 H15 . . 119.7
C16 C15 H15 . . 119.7
C17 C16 C15 . . 120.3(4)
C17 C16 Br2 . . 120.6(4)
C15 C16 Br2 . . 119.1(4)
C18 C17 C16 . . 118.1(4)
C18 C17 H17 . . 120.9
C16 C17 H17 . . 120.9
C17 C18 C19 . . 120.2(5)
C17 C18 Br1 . . 121.8(4)
C19 C18 Br1 . . 118.0(4)
N1 C19 C18 . . 121.1(4)
N1 C19 H19 . . 119.4
C18 C19 H19 . . 119.4
C19 N1 C15 . . 119.6(4)
C19 N1 Co1 . . 119.6(3)
C15 N1 Co1 . . 120.7(3)
C1 O1 Co1 . . 110.1(3)
C2 O2 Co1 . . 110.3(3)
O1 Co1 O1 4_676 . 180.0
O1 Co1 O2 4_676 . 92.94(12)
O1 Co1 O2 . . 87.06(12)
O1 Co1 O2 4_676 4_676 87.06(12)
O1 Co1 O2 . 4_676 92.94(12)
O2 Co1 O2 . 4_676 180.00(19)
O1 Co1 N1 4_676 4_676 91.51(13)
O1 Co1 N1 . 4_676 88.49(13)
O2 Co1 N1 . 4_676 89.80(14)
O2 Co1 N1 4_676 4_676 90.19(14)
O1 Co1 N1 4_676 . 88.49(13)
O1 Co1 N1 . . 91.51(13)
O2 Co1 N1 . . 90.20(14)
O2 Co1 N1 4_676 . 89.81(14)
N1 Co1 N1 4_676 . 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 . 1.332(5)
C1 C6 . 1.406(6)
C1 C2 . 1.431(6)
C2 O2 . 1.341(5)
C2 C3 . 1.424(6)
C3 C4 . 1.394(6)
C3 C7 . 1.526(6)
C4 C5 . 1.418(6)
C4 H4 . 0.9500
C5 C6 . 1.376(6)
C5 C11 . 1.524(6)
C6 H6 . 0.9500
C7 C10 . 1.538(6)
C7 C8 . 1.542(6)
C7 C9 . 1.546(6)
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 . 1.486(7)
C11 C12 . 1.502(7)
C11 C14 . 1.519(8)
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 . 1.347(6)
C15 C16 . 1.389(6)
C15 H15 . 0.9500
C16 C17 . 1.379(7)
C16 Br2 . 1.878(5)
C17 C18 . 1.370(7)
C17 H17 . 0.9500
C18 C19 . 1.387(6)
C18 Br1 . 1.881(5)
C19 N1 . 1.342(6)
C19 H19 . 0.9500
N1 Co1 . 1.975(3)
O1 Co1 . 1.889(3)
O2 Co1 . 1.895(3)
Co1 O1 4_676 1.889(3)
Co1 O2 4_676 1.895(3)
Co1 N1 4_676 1.975(3)
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_site_symmetry_4
_geom_torsion
O1 C1 C2 O2 . 0.3(5)
C6 C1 C2 O2 . -179.7(4)
O1 C1 C2 C3 . -179.5(4)
C6 C1 C2 C3 . 0.4(6)
O2 C2 C3 C4 . -179.7(4)
C1 C2 C3 C4 . 0.1(6)
O2 C2 C3 C7 . -1.2(6)
C1 C2 C3 C7 . 178.7(4)
C2 C3 C4 C5 . 0.5(6)
C7 C3 C4 C5 . -178.1(4)
C3 C4 C5 C6 . -1.6(7)
C3 C4 C5 C11 . 175.4(4)
C4 C5 C6 C1 . 2.1(6)
C11 C5 C6 C1 . -174.8(4)
O1 C1 C6 C5 . 178.3(4)
C2 C1 C6 C5 . -1.6(6)
C4 C3 C7 C10 . -3.2(6)
C2 C3 C7 C10 . 178.3(4)
C4 C3 C7 C8 . 116.5(5)
C2 C3 C7 C8 . -62.0(5)
C4 C3 C7 C9 . -122.7(4)
C2 C3 C7 C9 . 58.8(5)
C6 C5 C11 C13 . -12.5(6)
C4 C5 C11 C13 . 170.6(5)
C6 C5 C11 C12 . -133.0(5)
C4 C5 C11 C12 . 50.2(6)
C6 C5 C11 C14 . 110.3(6)
C4 C5 C11 C14 . -66.6(6)
N1 C15 C16 C17 . 0.5(7)
N1 C15 C16 Br2 . -176.6(3)
C15 C16 C17 C18 . 0.8(7)
Br2 C16 C17 C18 . 177.9(3)
C16 C17 C18 C19 . -2.0(7)
C16 C17 C18 Br1 . 178.7(3)
C17 C18 C19 N1 . 1.8(7)
Br1 C18 C19 N1 . -178.8(3)
C18 C19 N1 C15 . -0.4(6)
C18 C19 N1 Co1 . 179.7(3)
C16 C15 N1 C19 . -0.7(6)
C16 C15 N1 Co1 . 179.1(3)
C6 C1 O1 Co1 . 175.2(3)
C2 C1 O1 Co1 . -4.8(4)
C3 C2 O2 Co1 . -175.9(3)
C1 C2 O2 Co1 . 4.3(4)
C1 O1 Co1 O2 . 5.7(3)
C1 O1 Co1 O2 4_676 -174.3(3)
C1 O1 Co1 N1 4_676 -84.2(3)
C1 O1 Co1 N1 . 95.8(3)
C2 O2 Co1 O1 4_676 174.4(3)
C2 O2 Co1 O1 . -5.6(3)
C2 O2 Co1 N1 4_676 82.9(3)
C2 O2 Co1 N1 . -97.1(3)
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 -0.003 431 197 ' '

_cod_database_fobs_code 2108073
