#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:47:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180155 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/51/7105161.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7105161
loop_
_publ_author_name
'Berben, Louise A'
'Peters, Jonas C'
_publ_section_title
;
 Hydrogen evolution by cobalt tetraimine catalysts adsorbed on
 electrode surfaces.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              398
_journal_page_last               400
_journal_paper_doi               10.1039/b921559j
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C20 H22 B Br2 Co F2 N4 O2'
_chemical_formula_sum            'C20 H22 B Br2 Co F2 N4 O2'
_chemical_formula_weight         617.98
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.2153(8)
_cell_length_b                   13.1102(8)
_cell_length_c                   28.6077(18)
_cell_measurement_temperature    100(2)
_cell_volume                     4581.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  APEX2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            85831
_diffrn_reflns_theta_full        27.72
_diffrn_reflns_theta_max         27.72
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    4.279
_exptl_absorpt_correction_T_max  0.5662
_exptl_absorpt_correction_T_min  0.4143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta. Cryst.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0416P)²+3.2325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                4251
_reflns_number_total             5361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b921559j.txt
_cod_data_source_block           08113
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7105161
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.54006(3) 0.00860(3) 0.618873(14) 0.01268(10) Uani 1 1 d . . .
Br1 Br 0.55128(3) 0.13624(2) 0.678186(11) 0.01952(9) Uani 1 1 d . . .
Br2 Br 0.51361(3) -0.11509(2) 0.559629(11) 0.01843(9) Uani 1 1 d . . .
N1 N 0.6485(2) 0.0782(2) 0.58353(9) 0.0172(6) Uani 1 1 d . . .
N2 N 0.6421(2) -0.0821(2) 0.64729(9) 0.0164(5) Uani 1 1 d . . .
N3 N 0.4408(2) -0.06639(19) 0.66143(9) 0.0136(5) Uani 1 1 d . . .
N4 N 0.4455(2) 0.10468(19) 0.58449(8) 0.0128(5) Uani 1 1 d . . .
C1 C 0.1504(3) 0.1530(2) 0.60697(12) 0.0216(7) Uani 1 1 d . . .
H1 H 0.1051 0.1877 0.6288 0.026 Uiso 1 1 calc R . .
C2 C 0.1379(3) -0.0789(3) 0.65176(12) 0.0248(8) Uani 1 1 d . . .
H2 H 0.0836 -0.1080 0.6321 0.030 Uiso 1 1 calc R . .
C3 C 0.1685(3) 0.0535(3) 0.53703(12) 0.0213(7) Uani 1 1 d . . .
H3 H 0.1359 0.0191 0.5113 0.026 Uiso 1 1 calc R . .
C4 C 0.2965(3) 0.0054(2) 0.71026(11) 0.0222(7) Uani 1 1 d . . .
H4 H 0.3507 0.0340 0.7301 0.027 Uiso 1 1 calc R . .
C5 C 0.1031(3) 0.1034(3) 0.56932(12) 0.0228(7) Uani 1 1 d . . .
H5 H 0.0259 0.1035 0.5656 0.027 Uiso 1 1 calc R . .
C6 C 0.2484(3) -0.0905(2) 0.64079(11) 0.0177(6) Uani 1 1 d . . .
H6 H 0.2700 -0.1265 0.6135 0.021 Uiso 1 1 calc R . .
C7 C 0.1069(3) -0.0247(3) 0.69157(13) 0.0298(9) Uani 1 1 d . . .
H7 H 0.0316 -0.0163 0.6988 0.036 Uiso 1 1 calc R . .
C8 C 0.2815(3) 0.0537(2) 0.54220(11) 0.0169(6) Uani 1 1 d . . .
H8 H 0.3266 0.0204 0.5199 0.020 Uiso 1 1 calc R . .
C9 C 0.1859(3) 0.0168(3) 0.72045(12) 0.0284(8) Uani 1 1 d . . .
H9 H 0.1643 0.0536 0.7476 0.034 Uiso 1 1 calc R . .
C10 C 0.2629(3) 0.1528(2) 0.61324(11) 0.0181(6) Uani 1 1 d . . .
H10 H 0.2948 0.1858 0.6395 0.022 Uiso 1 1 calc R . .
C11 C 0.3283(2) 0.1034(2) 0.58050(10) 0.0136(6) Uani 1 1 d . . .
C12 C 0.3263(2) -0.0487(2) 0.67041(10) 0.0148(6) Uani 1 1 d . . .
C13 C 0.4998(2) 0.1749(2) 0.56260(10) 0.0146(6) Uani 1 1 d . . .
C14 C 0.4902(3) -0.1344(2) 0.68701(10) 0.0157(6) Uani 1 1 d . . .
C15 C 0.6194(3) 0.1596(2) 0.56108(11) 0.0172(6) Uani 1 1 d . . .
C16 C 0.6078(3) -0.1454(2) 0.67890(11) 0.0181(7) Uani 1 1 d . . .
C17 C 0.6954(3) 0.2266(3) 0.53472(12) 0.0237(7) Uani 1 1 d . . .
H17A H 0.7711 0.2096 0.5429 0.036 Uiso 1 1 calc R . .
H17B H 0.6808 0.2980 0.5427 0.036 Uiso 1 1 calc R . .
H17C H 0.6845 0.2165 0.5011 0.036 Uiso 1 1 calc R . .
C18 C 0.6773(3) -0.2228(3) 0.70249(12) 0.0253(8) Uani 1 1 d . . .
H18A H 0.6670 -0.2892 0.6874 0.038 Uiso 1 1 calc R . .
H18B H 0.6564 -0.2276 0.7355 0.038 Uiso 1 1 calc R . .
H18C H 0.7544 -0.2026 0.7002 0.038 Uiso 1 1 calc R . .
C19 C 0.4354(3) -0.2019(3) 0.72223(11) 0.0221(7) Uani 1 1 d . . .
H19A H 0.4547 -0.1792 0.7538 0.033 Uiso 1 1 calc R . .
H19B H 0.4599 -0.2724 0.7178 0.033 Uiso 1 1 calc R . .
H19C H 0.3559 -0.1982 0.7181 0.033 Uiso 1 1 calc R . .
C20 C 0.4517(3) 0.2664(2) 0.53946(11) 0.0174(6) Uani 1 1 d . . .
H20A H 0.3724 0.2674 0.5446 0.026 Uiso 1 1 calc R . .
H20B H 0.4667 0.2637 0.5058 0.026 Uiso 1 1 calc R . .
H20C H 0.4844 0.3282 0.5527 0.026 Uiso 1 1 calc R . .
O1 O 0.75411(18) 0.04922(18) 0.57819(8) 0.0248(5) Uani 1 1 d . . .
O2 O 0.74618(18) -0.09745(18) 0.63255(8) 0.0227(5) Uani 1 1 d . . .
B1 B 0.8086(3) -0.0074(3) 0.61662(14) 0.0217(8) Uani 1 1 d . . .
F1 F 0.82948(17) 0.05637(16) 0.65371(8) 0.0356(5) Uani 1 1 d . . .
F2 F 0.90306(16) -0.04614(15) 0.59701(8) 0.0303(5) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N2 94.02(11) . . ?
N1 Co1 N4 80.59(11) . . ?
N2 Co1 N4 174.23(11) . . ?
N1 Co1 N3 173.13(11) . . ?
N2 Co1 N3 80.12(11) . . ?
N4 Co1 N3 105.38(11) . . ?
N1 Co1 Br2 92.47(8) . . ?
N2 Co1 Br2 88.13(8) . . ?
N4 Co1 Br2 90.03(7) . . ?
N3 Co1 Br2 90.95(7) . . ?
N1 Co1 Br1 90.10(8) . . ?
N2 Co1 Br1 95.54(8) . . ?
N4 Co1 Br1 86.58(7) . . ?
N3 Co1 Br1 86.91(7) . . ?
Br2 Co1 Br1 175.37(2) . . ?
C15 N1 O1 115.9(3) . . ?
C15 N1 Co1 117.9(2) . . ?
O1 N1 Co1 126.2(2) . . ?
C16 N2 O2 115.2(3) . . ?
C16 N2 Co1 119.0(2) . . ?
O2 N2 Co1 125.05(19) . . ?
C14 N3 C12 117.4(3) . . ?
C14 N3 Co1 113.7(2) . . ?
C12 N3 Co1 128.62(19) . . ?
C13 N4 C11 118.7(3) . . ?
C13 N4 Co1 113.3(2) . . ?
C11 N4 Co1 128.02(19) . . ?
C5 C1 C10 120.9(3) . . ?
C7 C2 C6 120.1(3) . . ?
C5 C3 C8 120.1(3) . . ?
C9 C4 C12 118.7(3) . . ?
C1 C5 C3 120.0(3) . . ?
C12 C6 C2 118.9(3) . . ?
C9 C7 C2 120.0(3) . . ?
C3 C8 C11 119.4(3) . . ?
C7 C9 C4 120.7(3) . . ?
C1 C10 C11 118.9(3) . . ?
C10 C11 C8 120.7(3) . . ?
C10 C11 N4 120.9(3) . . ?
C8 C11 N4 118.4(3) . . ?
C6 C12 C4 121.5(3) . . ?
C6 C12 N3 119.5(3) . . ?
C4 C12 N3 118.8(3) . . ?
N4 C13 C15 115.1(3) . . ?
N4 C13 C20 125.8(3) . . ?
C15 C13 C20 119.1(3) . . ?
N3 C14 C16 115.7(3) . . ?
N3 C14 C19 125.1(3) . . ?
C16 C14 C19 119.2(3) . . ?
N1 C15 C13 111.7(3) . . ?
N1 C15 C17 124.6(3) . . ?
C13 C15 C17 123.6(3) . . ?
N2 C16 C14 111.4(3) . . ?
N2 C16 C18 124.7(3) . . ?
C14 C16 C18 123.8(3) . . ?
N1 O1 B1 118.9(2) . . ?
N2 O2 B1 117.5(2) . . ?
F1 B1 F2 112.5(3) . . ?
F1 B1 O2 110.1(3) . . ?
F2 B1 O2 105.3(3) . . ?
F1 B1 O1 110.5(3) . . ?
F2 B1 O1 104.9(3) . . ?
O2 B1 O1 113.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 1.900(3) . ?
Co1 N2 1.905(3) . ?
Co1 N4 1.972(2) . ?
Co1 N3 1.980(3) . ?
Co1 Br2 2.3678(5) . ?
Co1 Br1 2.3870(5) . ?
N1 C15 1.295(4) . ?
N1 O1 1.353(3) . ?
N2 C16 1.297(4) . ?
N2 O2 1.354(3) . ?
N3 C14 1.302(4) . ?
N3 C12 1.441(4) . ?
N4 C13 1.296(4) . ?
N4 C11 1.437(4) . ?
C1 C5 1.385(5) . ?
C1 C10 1.385(4) . ?
C2 C7 1.395(5) . ?
C2 C6 1.395(5) . ?
C3 C5 1.385(5) . ?
C3 C8 1.389(4) . ?
C4 C9 1.391(5) . ?
C4 C12 1.391(4) . ?
C6 C12 1.387(4) . ?
C7 C9 1.381(5) . ?
C8 C11 1.397(4) . ?
C10 C11 1.391(4) . ?
C13 C15 1.475(4) . ?
C13 C20 1.491(4) . ?
C14 C16 1.462(4) . ?
C14 C19 1.499(4) . ?
C15 C17 1.484(4) . ?
C16 C18 1.485(4) . ?
O1 B1 1.484(4) . ?
O2 B1 1.477(4) . ?
B1 F1 1.375(4) . ?
B1 F2 1.380(4) . ?
