#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:24:09 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178781 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/35/4103581.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_4103581
loop_
_publ_author_name
'Jaeheung Cho'
'Ritimukta Sarangi'
'Hye Yeon Kang'
'Jung Yoon Lee'
'Minoru Kubo'
'Takashi Ogura'
'Edward I. Solomon'
'Wonwoo Nam'
_publ_contact_author_address
; Department of Chemistry and Nano Science
  Ewha Womans University
  Seoul 120-750
  Korea
;
_publ_contact_author_email       jaeheung@ewha.ac.kr
_publ_contact_author_name        'Dr. Jaeheung Cho'
_publ_section_title
;
 Synthesis, Structural, and Spectroscopic Characterization and
 Reactivities of Mononuclear Cobalt(III)-Peroxo Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16977
_journal_page_last               16986
_journal_paper_doi               10.1021/ja107177m
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C14 H0 Cl2 Co N5 O8'
_chemical_formula_weight         524.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of form.cif'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.718(2)
_cell_length_b                   8.9472(12)
_cell_length_c                   17.545(2)
_cell_measurement_reflns_used    2381
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.89
_cell_measurement_theta_min      2.35
_cell_volume                     2310.4(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0966
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13894
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1266P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2227
_refine_ls_wR_factor_ref         0.2324
_reflns_number_gt                1569
_reflns_number_total             2927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107177m_si_002.cif
_cod_data_source_block           cho122pnma
_cod_database_code               4103581
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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 0.23426(7) 0.7500 0.59484(5) 0.0419(3) Uani 1 2 d S
Cl1 Cl 0.32264(17) 0.7500 0.88682(12) 0.0674(6) Uani 1 2 d S
Cl2 Cl 0.45310(13) 0.7500 0.32503(10) 0.0533(5) Uani 1 2 d S
N3 N 0.1875(5) 0.7500 0.4865(4) 0.0609(17) Uani 1 2 d S
N1 N 0.3319(3) 0.9022(5) 0.5896(2) 0.0541(11) Uani 1 1 d .
N2 N 0.1548(3) 0.9054(5) 0.6424(2) 0.0595(11) Uani 1 1 d .
O4 O 0.5006(5) 0.7500 0.3954(3) 0.106(3) Uani 1 2 d S
C7 C 0.1709(6) 0.7500 0.4210(5) 0.062(2) Uani 1 2 d S
O1 O 0.2283(6) 0.7500 0.8884(6) 0.179(5) Uani 1 2 d S
O6 O 0.4830(5) 0.8710(8) 0.2812(4) 0.156(3) Uani 1 1 d .
O5 O 0.3619(5) 0.7500 0.3329(5) 0.181(5) Uani 1 2 d S
C1 C 0.3511(5) 0.9739(7) 0.5141(3) 0.087(2) Uani 1 1 d .
C2 C 0.0875(6) 0.9785(9) 0.5945(4) 0.099(2) Uani 1 1 d .
C6 C 0.1107(7) 0.8271(7) 0.7068(4) 0.141(4) Uani 1 1 d .
C3 C 0.4141(6) 0.8272(8) 0.6156(6) 0.154(4) Uani 1 1 d .
O3 O 0.3484(10) 0.7500 0.9565(5) 0.229(7) Uani 1 2 d S
C4 C 0.3038(6) 1.0183(8) 0.6479(4) 0.110(3) Uani 1 1 d .
O2 O 0.3483(7) 0.8661(10) 0.8451(5) 0.267(6) Uani 1 1 d .
C5 C 0.2178(11) 0.9865(17) 0.6909(9) 0.070(4) Uani 0.50 1 d P
C5* C 0.2162(12) 1.0419(16) 0.6522(10) 0.072(4) Uani 0.50 1 d P
C8 C 0.1470(8) 0.7500 0.3383(5) 0.097(3) Uani 1 2 d S
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'
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'
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 86.8(3) 7_575 .
N1 Co1 N2 157.12(17) 7_575 .
N1 Co1 N2 88.01(18) . .
N1 Co1 N2 88.01(18) 7_575 7_575
N1 Co1 N2 157.12(17) . 7_575
N2 Co1 N2 88.1(3) . 7_575
N1 Co1 N3 101.72(18) 7_575 .
N1 Co1 N3 101.72(19) . .
N2 Co1 N3 101.16(19) . .
N2 Co1 N3 101.16(19) 7_575 .
O3 Cl1 O2 116.3(6) . 7_575
O3 Cl1 O2 116.3(6) . .
O2 Cl1 O2 103.2(11) 7_575 .
O3 Cl1 O1 106.1(8) . .
O2 Cl1 O1 107.2(6) 7_575 .
O2 Cl1 O1 107.2(6) . .
O5 Cl2 O6 111.6(4) . .
O5 Cl2 O6 111.6(4) . 7_575
O6 Cl2 O6 101.4(7) . 7_575
O5 Cl2 O4 113.7(5) . .
O6 Cl2 O4 108.9(4) . .
O6 Cl2 O4 108.9(4) 7_575 .
C7 N3 Co1 172.1(7) . .
C3 N1 C1 108.5(6) . .
C3 N1 C4 109.4(6) . .
C1 N1 C4 110.8(5) . .
C3 N1 Co1 105.7(4) . .
C1 N1 Co1 118.1(3) . .
C4 N1 Co1 104.0(4) . .
C2 N2 C5 123.2(8) . .
C2 N2 C6 110.8(6) . .
C5 N2 C6 93.9(8) . .
C2 N2 C5* 96.2(8) . .
C5 N2 C5* 32.6(7) . .
C6 N2 C5* 123.4(8) . .
C2 N2 Co1 118.1(4) . .
C5 N2 Co1 102.7(7) . .
C6 N2 Co1 104.3(3) . .
C5* N2 Co1 104.9(7) . .
N3 C7 C8 178.4(9) . .
C6 C6 N2 118.2(3) 7_575 .
C3 C3 N1 117.5(3) 7_575 .
C5* C4 C5 34.0(8) . .
C5* C4 N1 114.8(9) . .
C5 C4 N1 116.1(7) . .
C5* C5 C4 60.4(18) . .
C5* C5 N2 78.7(19) . .
C4 C5 N2 109.7(10) . .
C5 C5* C4 86(2) . .
C5 C5* N2 68.7(17) . .
C4 C5* N2 116.5(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 1.982(4) 7_575
Co1 N1 1.982(4) .
Co1 N2 1.998(4) .
Co1 N2 1.999(4) 7_575
Co1 N3 2.022(6) .
Cl1 O3 1.281(8) .
Cl1 O2 1.326(7) 7_575
Cl1 O2 1.326(7) .
Cl1 O1 1.389(9) .
Cl2 O5 1.349(7) .
Cl2 O6 1.399(6) .
Cl2 O6 1.399(6) 7_575
Cl2 O4 1.420(6) .
N3 C7 1.173(9) .
N1 C3 1.457(8) .
N1 C1 1.498(7) .
N1 C4 1.515(7) .
N2 C2 1.454(8) .
N2 C5 1.453(16) .
N2 C6 1.480(7) .
N2 C5* 1.529(16) .
C7 C8 1.494(11) .
C6 C6 1.379(13) 7_575
C3 C3 1.381(15) 7_575
C4 C5* 1.308(19) .
C4 C5 1.501(17) .
C5 C5* 0.841(17) .
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 N3 C7 -44.58(14) 7_575 .
N1 Co1 N3 C7 44.58(14) . .
N2 Co1 N3 C7 134.85(13) . .
N2 Co1 N3 C7 -134.85(13) 7_575 .
N1 Co1 N1 C3 -22.2(6) 7_575 .
N2 Co1 N1 C3 135.5(5) . .
N2 Co1 N1 C3 55.0(7) 7_575 .
N3 Co1 N1 C3 -123.6(5) . .
N1 Co1 N1 C1 99.3(4) 7_575 .
N2 Co1 N1 C1 -103.0(4) . .
N2 Co1 N1 C1 176.6(5) 7_575 .
N3 Co1 N1 C1 -2.0(5) . .
N1 Co1 N1 C4 -137.4(4) 7_575 .
N2 Co1 N1 C4 20.3(5) . .
N2 Co1 N1 C4 -60.2(7) 7_575 .
N3 Co1 N1 C4 121.2(5) . .
N1 Co1 N2 C2 178.4(5) 7_575 .
N1 Co1 N2 C2 101.4(5) . .
N2 Co1 N2 C2 -101.2(5) 7_575 .
N3 Co1 N2 C2 -0.2(5) . .
N1 Co1 N2 C5 39.3(9) 7_575 .
N1 Co1 N2 C5 -37.7(7) . .
N2 Co1 N2 C5 119.7(7) 7_575 .
N3 Co1 N2 C5 -139.3(7) . .
N1 Co1 N2 C6 -58.2(7) 7_575 .
N1 Co1 N2 C6 -135.2(5) . .
N2 Co1 N2 C6 22.2(6) 7_575 .
N3 Co1 N2 C6 123.2(5) . .
N1 Co1 N2 C5* 72.8(8) 7_575 .
N1 Co1 N2 C5* -4.2(7) . .
N2 Co1 N2 C5* 153.2(7) 7_575 .
N3 Co1 N2 C5* -105.8(7) . .
Co1 N3 C7 C8 180.00(5) . .
C2 N2 C6 C6 110.0(4) . 7_575
C5 N2 C6 C6 -122.1(7) . 7_575
C5* N2 C6 C6 -137.1(8) . 7_575
Co1 N2 C6 C6 -18.0(4) . 7_575
C1 N1 C3 C3 -109.6(4) . 7_575
C4 N1 C3 C3 129.5(4) . 7_575
Co1 N1 C3 C3 18.1(5) . 7_575
C3 N1 C4 C5* -149.2(11) . .
C1 N1 C4 C5* 91.3(11) . .
Co1 N1 C4 C5* -36.6(11) . .
C3 N1 C4 C5 -111.5(12) . .
C1 N1 C4 C5 129.0(11) . .
Co1 N1 C4 C5 1.1(12) . .
N1 C4 C5 C5* -96.2(19) . .
C5* C4 C5 N2 63.6(17) . .
N1 C4 C5 N2 -32.6(16) . .
C2 N2 C5 C5* -38(2) . .
C6 N2 C5 C5* -156.5(18) . .
Co1 N2 C5 C5* 98.0(19) . .
C2 N2 C5 C4 -91.0(12) . .
C6 N2 C5 C4 151.0(11) . .
C5* N2 C5 C4 -52.6(15) . .
Co1 N2 C5 C4 45.4(12) . .
N2 C5 C5* C4 -120.7(8) . .
C4 C5 C5* N2 120.7(8) . .
N1 C4 C5* C5 100.5(18) . .
C5 C4 C5* N2 -63.6(15) . .
N1 C4 C5* N2 36.9(17) . .
C2 N2 C5* C5 148.5(18) . .
C6 N2 C5* C5 29(2) . .
Co1 N2 C5* C5 -90.3(19) . .
C2 N2 C5* C4 -138.1(13) . .
C5 N2 C5* C4 73(2) . .
C6 N2 C5* C4 102.0(14) . .
Co1 N2 C5* C4 -16.8(15) . .
