#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/22/4102270.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_4102270
loop_
_publ_author_name
'J. Krzystek'
'Dale C. Swenson'
'S. A. Zvyagin'
'Dmitry Smirnov'
'Andrew Ozarowski'
'Joshua Telser'
_publ_section_title
;
 Cobalt(II) "Scorpionate" Complexes as Models for Cobalt-Substituted Zinc
 Enzymes: Electronic Structure Investigation by High-Frequency and -Field
 Electron Paramagnetic Resonance Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5241
_journal_page_last               5253
_journal_paper_doi               10.1021/ja910766w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C24 H40 B Cl Co N6'
_chemical_formula_sum            'C24 H40 B Cl Co N6'
_chemical_formula_weight         517.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.9843(17)
_cell_length_b                   15.9843(17)
_cell_length_c                   9.4269(10)
_cell_measurement_reflns_used    2665
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     2085.9(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo, Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL v6.1 (Sheldrick, 1997)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD phi and omega scans'
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9505
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_correction_T_min  0.8095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             825
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.442(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1175
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0297P)²+0.7201P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                1148
_reflns_number_total             1175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910766w_si_002_5.cif
_cod_data_source_block           Tp(t-Bu)(Me)CoCl
_cod_original_sg_symbol_Hall     ' R 3 -2" '
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4102270
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
Co1 Co 1.0000 1.0000 0.84653(5) 0.02105(12) Uani 1 6 d S
Cl1 Cl 1.0000 1.0000 1.08204(11) 0.0353(2) Uani 1 6 d S
N1 N 0.93751(6) 0.87501(13) 0.73403(18) 0.0252(4) Uani 1 2 d S
N2 N 0.94730(6) 0.89461(13) 0.59076(17) 0.0242(4) Uani 1 2 d S
B1 B 1.0000 1.0000 0.5351(4) 0.0232(8) Uani 1 6 d SD
H1 H 1.0000 1.0000 0.4290(4) 0.028 Uiso 1 6 d SD
C2 C 0.88947(8) 0.77894(16) 0.7489(2) 0.0345(5) Uani 1 2 d S
C3 C 0.86824(9) 0.73649(18) 0.6150(3) 0.0445(6) Uani 1 2 d S
H3 H 0.8346 0.6693 0.5946 0.053 Uiso 1 2 calc SR
C4 C 0.90534(8) 0.81069(17) 0.5178(2) 0.0326(5) Uani 1 2 d S
C5 C 0.86489(9) 0.72978(17) 0.8932(3) 0.0452(7) Uani 1 2 d S
C6 C 0.81007(11) 0.6201(2) 0.8712(4) 0.0937(16) Uani 1 2 d S
H6A H 0.7939 0.5877 0.9636 0.141 Uiso 1 2 calc SR
H6B H 0.8507 0.6013 0.8179 0.141 Uiso 0.50 1 calc PR
H6C H 0.7506 0.6013 0.8180 0.141 Uiso 0.50 1 calc PR
C7 C 0.95832(17) 0.75886(16) 0.9753(2) 0.0517(5) Uani 1 1 d .
H7A H 0.9987 0.7402 0.9209 0.078 Uiso 1 1 calc R
H7B H 0.9425 0.7260 1.0674 0.078 Uiso 1 1 calc R
H7C H 0.9935 0.8289 0.9900 0.078 Uiso 1 1 calc R
C23 C 0.90294(10) 0.8059(2) 0.3588(3) 0.0440(6) Uani 1 2 d S
H23A H 0.9358 0.8715 0.3198 0.066 Uiso 0.50 2 calc SPR
H23B H 0.8357 0.7715 0.3264 0.066 Uiso 0.25 1 calc PR
H23C H 0.9358 0.7715 0.3264 0.066 Uiso 0.25 1 calc PR
H23D H 0.8691 0.7381 0.3286 0.066 Uiso 0.50 2 calc SPR
H23E H 0.9691 0.8382 0.3220 0.066 Uiso 0.25 1 calc PR
H23F H 0.8690 0.8382 0.3220 0.066 Uiso 0.25 1 calc PR
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'
Cl Cl 0.1484 0.1585 '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'
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
N1 Co1 N1 95.18(7) 3_675 2_765
N1 Co1 N1 95.18(7) 3_675 .
N1 Co1 N1 95.18(7) 2_765 .
N1 Co1 Cl1 121.51(5) 3_675 .
N1 Co1 Cl1 121.51(5) 2_765 .
N1 Co1 Cl1 121.51(5) . .
C2 N1 N2 107.36(17) . .
C2 N1 Co1 142.49(15) . .
N2 N1 Co1 110.15(13) . .
C4 N2 N1 109.27(17) . .
C4 N2 B1 129.6(2) . .
N1 N2 B1 121.1(2) . .
N2 B1 N2 109.16(16) 3_675 2_765
N2 B1 N2 109.16(16) 3_675 .
N2 B1 N2 109.16(16) 2_765 .
N2 B1 H1 109.78(16) 3_675 .
N2 B1 H1 109.78(16) 2_765 .
N2 B1 H1 109.78(15) . .
N1 C2 C3 109.0(2) . .
N1 C2 C5 122.6(2) . .
C3 C2 C5 128.5(2) . .
C4 C3 C2 106.8(2) . .
C4 C3 H3 126.6 . .
C2 C3 H3 126.6 . .
N2 C4 C3 107.66(19) . .
N2 C4 C23 123.2(2) . .
C3 C4 C23 129.2(2) . .
C2 C5 C6 108.8(3) . .
C2 C5 C7 109.51(13) . 5_655
C6 C5 C7 109.17(15) . 5_655
C2 C5 C7 109.51(13) . .
C6 C5 C7 109.17(15) . .
C7 C5 C7 110.7(2) 5_655 .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C4 C23 H23A 109.5 . .
C4 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C4 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C4 C23 H23D 109.5 . .
H23A C23 H23D 141.1 . .
H23B C23 H23D 56.3 . .
H23C C23 H23D 56.3 . .
C4 C23 H23E 109.5 . .
H23A C23 H23E 56.3 . .
H23B C23 H23E 141.1 . .
H23C C23 H23E 56.3 . .
H23D C23 H23E 109.5 . .
C4 C23 H23F 109.5 . .
H23A C23 H23F 56.3 . .
H23B C23 H23F 56.3 . .
H23C C23 H23F 141.1 . .
H23D C23 H23F 109.5 . .
H23E C23 H23F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.0293(17) 3_675
Co1 N1 2.0293(18) 2_765
Co1 N1 2.0293(17) .
Co1 Cl1 2.2202(10) .
N1 C2 1.337(3) .
N1 N2 1.378(2) .
N2 C4 1.350(3) .
N2 B1 1.550(2) .
B1 N2 1.550(2) 3_675
B1 N2 1.550(2) 2_765
B1 H1 1.0001(10) .
C2 C3 1.392(4) .
C2 C5 1.521(3) .
C3 C4 1.376(3) .
C3 H3 0.9500 .
C4 C23 1.500(3) .
C5 C6 1.532(4) .
C5 C7 1.533(3) 5_655
C5 C7 1.533(3) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C23 H23D 0.9800 .
C23 H23E 0.9800 .
C23 H23F 0.9800 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Co1 N1 C2 -132.15(4) 3_675 .
N1 Co1 N1 C2 132.15(4) 2_765 .
Cl1 Co1 N1 C2 0.000(1) . .
N1 Co1 N1 N2 47.85(4) 3_675 .
N1 Co1 N1 N2 -47.85(4) 2_765 .
Cl1 Co1 N1 N2 180.0 . .
C2 N1 N2 C4 0.000(1) . .
Co1 N1 N2 C4 180.0 . .
C2 N1 N2 B1 180.000(1) . .
Co1 N1 N2 B1 0.000(1) . .
C4 N2 B1 N2 120.38(19) . 3_675
N1 N2 B1 N2 -59.62(19) . 3_675
C4 N2 B1 N2 -120.38(19) . 2_765
N1 N2 B1 N2 59.62(19) . 2_765
N2 N1 C2 C3 0.000(1) . .
Co1 N1 C2 C3 180.000(1) . .
N2 N1 C2 C5 180.000(1) . .
Co1 N1 C2 C5 0.000(2) . .
N1 C2 C3 C4 0.000(1) . .
C5 C2 C3 C4 180.000(1) . .
N1 N2 C4 C3 0.000(1) . .
B1 N2 C4 C3 180.0 . .
N1 N2 C4 C23 180.000(1) . .
B1 N2 C4 C23 0.000(1) . .
C2 C3 C4 N2 0.000(1) . .
C2 C3 C4 C23 180.000(1) . .
N1 C2 C5 C6 180.000(1) . .
C3 C2 C5 C6 0.000(2) . .
N1 C2 C5 C7 60.75(15) . 5_655
C3 C2 C5 C7 -119.25(15) . 5_655
N1 C2 C5 C7 -60.75(15) . .
C3 C2 C5 C7 119.25(15) . .
