#------------------------------------------------------------------------------
#$Date: 2017-07-25 11:46:04 +0300 (Tue, 25 Jul 2017) $
#$Revision: 199049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/80/2108070.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_2108070
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      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
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                86.394(4)
_cell_angle_beta                 89.775(5)
_cell_angle_gamma                65.652(4)
_cell_formula_units_Z            1
_cell_length_a                   9.0047(11)
_cell_length_b                   10.2138(12)
_cell_length_c                   11.6756(14)
_cell_measurement_reflns_used    18550
_cell_measurement_temperature    235(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      1.37
_cell_volume                     976.1(2)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      235(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.961
_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  0.0493
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18550
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.520
_diffrn_reflns_theta_min         1.379
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS, 2008'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             487
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.986
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0455
_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)+(0.0840P)²+0.2837P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1494
_reflns_number_gt                2784
_reflns_number_total             3840
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ps5056sup1.cif
_cod_data_source_block           1_235K
_cod_database_code               2108070
_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.
;
_shelxl_version_number           201.4
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
C C1 0.9462(5) 0.6147(4) 0.7026(3) 0.0265(9) Uani d 1
C C2 0.8149(5) 0.5754(4) 0.6844(4) 0.0272(9) Uani d 1
C C3 0.6871(6) 0.6077(4) 0.7651(4) 0.0320(10) Uani d 1
C C4 0.7033(6) 0.6763(5) 0.8608(4) 0.0354(11) Uani d 1
H H4 0.6202 0.7005 0.9149 0.042 Uiso calc 1
C C5 0.8354(6) 0.7115(5) 0.8817(4) 0.0339(10) Uani d 1
C C6 0.9570(6) 0.6815(5) 0.8014(4) 0.0328(10) Uani d 1
H H6 1.0456 0.7057 0.8132 0.039 Uiso calc 1
C C7 0.5489(6) 0.5605(5) 0.7507(4) 0.0379(11) Uani d 1
C C8 0.4643(7) 0.6105(6) 0.6328(5) 0.0471(13) Uani d 1
H H8A 0.3680 0.5906 0.6306 0.071 Uiso calc 1
H H8B 0.5385 0.5595 0.5741 0.071 Uiso calc 1
H H8C 0.4328 0.7132 0.6188 0.071 Uiso calc 1
C C9 0.6157(8) 0.3958(6) 0.7636(6) 0.0628(17) Uani d 1
H H9A 0.6616 0.3620 0.8404 0.094 Uiso calc 1
H H9B 0.6997 0.3549 0.7078 0.094 Uiso calc 1
H H9C 0.5280 0.3662 0.7506 0.094 Uiso calc 1
C C10 0.4167(7) 0.6215(7) 0.8414(5) 0.0521(14) Uani d 1
H H10A 0.4652 0.5881 0.9176 0.078 Uiso calc 1
H H10B 0.3312 0.5889 0.8297 0.078 Uiso calc 1
H H10C 0.3709 0.7259 0.8337 0.078 Uiso calc 1
C C11 0.8440(7) 0.7825(5) 0.9934(4) 0.0417(12) Uani d 1
C C12 0.7848(16) 0.7185(11) 1.0935(6) 0.120(4) Uani d 1
H H12A 0.8181 0.7440 1.1647 0.179 Uiso calc 1
H H12B 0.8314 0.6145 1.0913 0.179 Uiso calc 1
H H12C 0.6668 0.7556 1.0891 0.179 Uiso calc 1
C C13 1.0179(11) 0.7550(14) 1.0246(8) 0.131(5) Uani d 1
H H13A 1.0564 0.8086 0.9698 0.197 Uiso calc 1
H H13B 1.0867 0.6529 1.0231 0.197 Uiso calc 1
H H13C 1.0219 0.7858 1.1010 0.197 Uiso calc 1
C C14 0.7440(14) 0.9425(8) 0.9776(7) 0.120(4) Uani d 1
H H14A 0.7639 0.9888 1.0422 0.180 Uiso calc 1
H H14B 0.6292 0.9618 0.9731 0.180 Uiso calc 1
H H14C 0.7745 0.9799 0.9072 0.180 Uiso calc 1
C C15 0.7082(6) 0.7398(5) 0.4135(4) 0.0337(10) Uani d 1
H H15 0.6589 0.6758 0.4298 0.040 Uiso calc 1
C C16 0.6138(6) 0.8798(5) 0.3690(4) 0.0364(11) Uani d 1
C C17 0.6847(6) 0.9723(5) 0.3416(4) 0.0385(12) Uani d 1
H H17 0.6232 1.0657 0.3088 0.046 Uiso calc 1
C C18 0.8501(6) 0.9241(5) 0.3638(4) 0.0386(11) Uani d 1
C C19 0.9385(6) 0.7870(5) 0.4109(4) 0.0359(11) Uani d 1
H H19 1.0502 0.7566 0.4279 0.043 Uiso calc 1
N N1 0.8681(5) 0.6960(4) 0.4330(3) 0.0308(8) Uani d 1
O O1 1.0603(4) 0.5815(3) 0.6234(2) 0.0293(7) Uani d 1
O O2 0.8199(4) 0.5084(3) 0.5896(3) 0.0300(7) Uani d 1
Co Co1 1.0000 0.5000 0.5000 0.0253(2) Uani d 1
Br Br1 0.95517(8) 1.04641(6) 0.32996(7) 0.0669(2) Uani d 1
Br Br2 0.38695(7) 0.94016(6) 0.34839(5) 0.0533(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 . . 121.8(4)
O1 C1 C2 . . 117.0(4)
C6 C1 C2 . . 121.1(4)
O2 C2 C1 . . 116.0(3)
O2 C2 C3 . . 123.5(4)
C1 C2 C3 . . 120.5(4)
C4 C3 C2 . . 115.7(4)
C4 C3 C7 . . 122.6(4)
C2 C3 C7 . . 121.6(4)
C3 C4 C5 . . 124.4(4)
C6 C5 C4 . . 119.1(4)
C6 C5 C11 . . 120.9(5)
C4 C5 C11 . . 119.9(4)
C5 C6 C1 . . 119.1(5)
C3 C7 C8 . . 111.8(4)
C3 C7 C9 . . 109.9(4)
C8 C7 C9 . . 108.0(5)
C3 C7 C10 . . 111.9(4)
C8 C7 C10 . . 107.1(4)
C9 C7 C10 . . 108.0(4)
C12 C11 C14 . . 110.6(7)
C12 C11 C13 . . 105.6(7)
C14 C11 C13 . . 108.9(8)
C12 C11 C5 . . 110.7(5)
C14 C11 C5 . . 109.5(5)
C13 C11 C5 . . 111.4(4)
N1 C15 C16 . . 120.5(5)
C17 C16 C15 . . 120.3(5)
C17 C16 Br2 . . 120.4(4)
C15 C16 Br2 . . 119.3(4)
C16 C17 C18 . . 117.7(4)
C19 C18 C17 . . 120.4(5)
C19 C18 Br1 . . 119.5(4)
C17 C18 Br1 . . 120.0(4)
N1 C19 C18 . . 120.9(5)
C15 N1 C19 . . 120.0(4)
C15 N1 Co1 . . 120.4(3)
C19 N1 Co1 . . 119.5(3)
C1 O1 Co1 . . 109.8(3)
C2 O2 Co1 . . 110.3(3)
O1 Co1 O1 2_766 . 180.00(17)
O1 Co1 O2 2_766 . 93.45(13)
O1 Co1 O2 . . 86.54(13)
O1 Co1 O2 2_766 2_766 86.54(13)
O1 Co1 O2 . 2_766 93.46(13)
O2 Co1 O2 . 2_766 180.0
O1 Co1 N1 2_766 . 91.00(14)
O1 Co1 N1 . . 89.00(14)
O2 Co1 N1 . . 89.60(13)
O2 Co1 N1 2_766 . 90.40(13)
O1 Co1 N1 2_766 2_766 89.00(14)
O1 Co1 N1 . 2_766 91.00(14)
O2 Co1 N1 . 2_766 90.40(13)
O2 Co1 N1 2_766 2_766 89.60(13)
N1 Co1 N1 . 2_766 180.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 O1 . 1.330(5)
C1 C6 . 1.401(6)
C1 C2 . 1.417(7)
C2 O2 . 1.329(5)
C2 C3 . 1.428(6)
C3 C4 . 1.394(7)
C3 C7 . 1.522(7)
C4 C5 . 1.403(7)
C5 C6 . 1.387(6)
C5 C11 . 1.550(7)
C7 C8 . 1.529(8)
C7 C9 . 1.532(7)
C7 C10 . 1.545(6)
C11 C12 . 1.505(9)
C11 C14 . 1.505(8)
C11 C13 . 1.514(10)
C15 N1 . 1.335(6)
C15 C16 . 1.394(6)
C16 C17 . 1.364(7)
C16 Br2 . 1.886(5)
C17 C18 . 1.381(7)
C18 C19 . 1.373(6)
C18 Br1 . 1.877(5)
C19 N1 . 1.337(6)
N1 Co1 . 1.970(4)
O1 Co1 . 1.896(3)
O2 Co1 . 1.901(3)
Co1 O1 2_766 1.896(3)
Co1 O2 2_766 1.901(3)
Co1 N1 2_766 1.970(4)
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 . -177.8(4)
O1 C1 C2 C3 . -179.7(3)
C6 C1 C2 C3 . 2.2(6)
O2 C2 C3 C4 . 178.9(4)
C1 C2 C3 C4 . -1.1(6)
O2 C2 C3 C7 . 3.0(6)
C1 C2 C3 C7 . -177.0(4)
C2 C3 C4 C5 . -1.0(6)
C7 C3 C4 C5 . 174.8(4)
C3 C4 C5 C6 . 2.2(7)
C3 C4 C5 C11 . -177.7(4)
C4 C5 C6 C1 . -1.1(6)
C11 C5 C6 C1 . 178.8(4)
O1 C1 C6 C5 . -179.0(4)
C2 C1 C6 C5 . -1.0(6)
C4 C3 C7 C8 . 130.5(5)
C2 C3 C7 C8 . -53.9(5)
C4 C3 C7 C9 . -109.6(5)
C2 C3 C7 C9 . 66.0(6)
C4 C3 C7 C10 . 10.4(6)
C2 C3 C7 C10 . -174.1(4)
C6 C5 C11 C12 . -141.2(7)
C4 C5 C11 C12 . 38.7(8)
C6 C5 C11 C14 . 96.6(7)
C4 C5 C11 C14 . -83.5(7)
C6 C5 C11 C13 . -23.9(8)
C4 C5 C11 C13 . 155.9(7)
N1 C15 C16 C17 . 2.0(7)
N1 C15 C16 Br2 . -177.5(3)
C15 C16 C17 C18 . -2.5(7)
Br2 C16 C17 C18 . 176.9(4)
C16 C17 C18 C19 . 0.6(7)
C16 C17 C18 Br1 . -179.3(3)
C17 C18 C19 N1 . 2.1(7)
Br1 C18 C19 N1 . -178.1(3)
C16 C15 N1 C19 . 0.6(6)
C16 C15 N1 Co1 . 178.2(3)
C18 C19 N1 C15 . -2.6(7)
C18 C19 N1 Co1 . 179.8(3)
C6 C1 O1 Co1 . -177.7(3)
C2 C1 O1 Co1 . 4.3(4)
C1 C2 O2 Co1 . -4.6(4)
C3 C2 O2 Co1 . 175.3(3)
C1 O1 Co1 O2 . -5.4(3)
C1 O1 Co1 O2 2_766 174.6(3)
C1 O1 Co1 N1 . 84.3(3)
C1 O1 Co1 N1 2_766 -95.7(3)

_cod_database_fobs_code 2108070
