#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:23:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180010 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/04/7030444.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_7030444
loop_
_publ_author_name
'Nebe, Thomas'
'Beitat, Alexander'
'Würtele, Christian'
'Dücker-Benfer, Carlos'
'van Eldik, Rudi'
'McKenzie, Christine J.'
'Schindler, Siegfried'
_publ_section_title
;
 Reinvestigation of the formation of a mononuclear Fe(III) hydroperoxido
 complex using high pressure kinetics.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7768
_journal_page_last               7773
_journal_paper_doi               10.1039/c0dt00247j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C21 H25 Cl Co F6 N5 Sb'
_chemical_formula_weight         677.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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            4
_cell_length_a                   18.260(4)
_cell_length_b                   9.1630(18)
_cell_length_c                   15.057(3)
_cell_measurement_temperature    193(2)
_cell_volume                     2519.3(9)
_computing_cell_refinement       'STOE IPDS Software (1997)'
_computing_data_collection       'STOE IPDS Software (1997)'
_computing_data_reduction        'STOE IPDS Software (1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'STOE IPDS'
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20623
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6001
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0357
_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)+(0.0640P)²+0.3112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                5449
_reflns_number_total             6001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00247j.txt
_cod_data_source_block           shin172sa
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7030444
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, 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
C1 C 0.0740(3) 0.7602(6) 0.8247(3) 0.0589(13) Uani 1 1 d .
H1A H 0.0454 0.8514 0.8315 0.071 Uiso 1 1 calc R
H1B H 0.0643 0.6978 0.8770 0.071 Uiso 1 1 calc R
C2 C 0.0504(2) 0.6826(5) 0.7422(3) 0.0454(9) Uani 1 1 d .
C3 C -0.0219(3) 0.6738(7) 0.7156(4) 0.0626(14) Uani 1 1 d .
H3 H -0.0588 0.7222 0.7489 0.075 Uiso 1 1 calc R
C4 C -0.0402(3) 0.5971(6) 0.6429(4) 0.0608(14) Uani 1 1 d .
H4 H -0.0900 0.5903 0.6249 0.073 Uiso 1 1 calc R
C5 C 0.0145(3) 0.5277(6) 0.5940(3) 0.0524(11) Uani 1 1 d .
H5 H 0.0030 0.4756 0.5413 0.063 Uiso 1 1 calc R
C6 C 0.0857(2) 0.5367(5) 0.6243(2) 0.0372(7) Uani 1 1 d .
H6 H 0.1232 0.4866 0.5929 0.045 Uiso 1 1 calc R
C7 C 0.1659(4) 0.9135(4) 0.7567(3) 0.0585(14) Uani 1 1 d .
H7A H 0.1580 1.0087 0.7862 0.070 Uiso 1 1 calc R
H7B H 0.1309 0.9058 0.7067 0.070 Uiso 1 1 calc R
C8 C 0.2411(4) 0.9058(4) 0.7227(3) 0.0552(14) Uani 1 1 d .
C9 C 0.2821(5) 1.0278(6) 0.7002(4) 0.084(2) Uani 1 1 d .
H9 H 0.2617 1.1226 0.7069 0.100 Uiso 1 1 calc R
C10 C 0.3508(5) 1.0122(8) 0.6687(4) 0.104(4) Uani 1 1 d .
H10 H 0.3791 1.0957 0.6539 0.125 Uiso 1 1 calc R
C11 C 0.3793(5) 0.8755(10) 0.6584(3) 0.088(3) Uani 1 1 d .
H11 H 0.4277 0.8625 0.6365 0.105 Uiso 1 1 calc R
C12 C 0.3366(3) 0.7563(6) 0.6806(3) 0.0534(11) Uani 1 1 d .
H12 H 0.3563 0.6611 0.6733 0.064 Uiso 1 1 calc R
C13 C 0.1856(3) 0.8272(5) 0.9075(3) 0.0539(11) Uani 1 1 d .
H13A H 0.1500 0.8809 0.9449 0.065 Uiso 1 1 calc R
H13B H 0.2292 0.8899 0.8993 0.065 Uiso 1 1 calc R
C14 C 0.2076(3) 0.6873(5) 0.9536(2) 0.0470(9) Uani 1 1 d .
H14A H 0.2340 0.7106 1.0092 0.056 Uiso 1 1 calc R
H14B H 0.1632 0.6308 0.9692 0.056 Uiso 1 1 calc R
C15 C 0.3310(3) 0.6509(6) 0.8954(3) 0.0533(11) Uani 1 1 d .
H15A H 0.3488 0.6556 0.9567 0.080 Uiso 1 1 calc R
H15B H 0.3328 0.7485 0.8689 0.080 Uiso 1 1 calc R
H15C H 0.3620 0.5843 0.8610 0.080 Uiso 1 1 calc R
C16 C 0.2548(2) 0.4454(4) 0.9272(3) 0.0411(8) Uani 1 1 d .
H16A H 0.2654 0.4444 0.9916 0.049 Uiso 1 1 calc R
H16B H 0.2938 0.3895 0.8967 0.049 Uiso 1 1 calc R
C17 C 0.1832(2) 0.3739(4) 0.9110(2) 0.0349(7) Uani 1 1 d .
C18 C 0.1577(2) 0.2622(4) 0.9659(3) 0.0411(8) Uani 1 1 d .
H18 H 0.1856 0.2314 1.0157 0.049 Uiso 1 1 calc R
C19 C 0.0923(3) 0.1978(5) 0.9470(3) 0.0488(10) Uani 1 1 d .
H19 H 0.0736 0.1229 0.9843 0.059 Uiso 1 1 calc R
C20 C 0.0534(3) 0.2421(5) 0.8736(3) 0.0486(9) Uani 1 1 d .
H20 H 0.0079 0.1981 0.8589 0.058 Uiso 1 1 calc R
C21 C 0.0823(2) 0.3523(5) 0.8218(3) 0.0453(9) Uani 1 1 d .
H21 H 0.0561 0.3816 0.7704 0.054 Uiso 1 1 calc R
Cl1 Cl 0.26686(5) 0.41919(9) 0.68569(8) 0.0414(2) Uani 1 1 d .
Co1 Co 0.20438(2) 0.59800(4) 0.76507(3) 0.02511(10) Uani 1 1 d .
F1 F 0.4065(4) -0.0960(4) 0.0438(4) 0.121(3) Uani 1 1 d .
F2 F 0.50723(18) 0.1013(4) 0.0057(3) 0.0792(10) Uani 1 1 d .
F3 F 0.4184(2) 0.0106(5) -0.1143(2) 0.0845(11) Uani 1 1 d .
F4 F 0.4081(2) 0.2760(4) -0.0488(4) 0.0898(12) Uani 1 1 d .
F5 F 0.3049(2) 0.0827(7) -0.0157(7) 0.151(3) Uani 1 1 d .
F6 F 0.3962(3) 0.1658(5) 0.1115(3) 0.1143(19) Uani 1 1 d .
N1 N 0.1524(2) 0.7950(4) 0.8203(2) 0.0452(8) Uani 1 1 d .
N2 N 0.10376(17) 0.6149(4) 0.6974(2) 0.0339(6) Uani 1 1 d .
N3 N 0.2690(2) 0.7710(3) 0.71158(19) 0.0412(8) Uani 1 1 d .
N4 N 0.2555(2) 0.5978(3) 0.8948(2) 0.0356(6) Uani 1 1 d .
N5 N 0.14509(19) 0.4194(3) 0.8404(2) 0.0364(7) Uani 1 1 d .
Sb1 Sb 0.404201(15) 0.08824(3) -0.001728(19) 0.04439(9) 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'
N N 0.0061 0.0033 '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'
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'
Sb Sb -0.5866 1.5461 '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
N1 C1 C2 110.2(3)
N2 C2 C3 121.5(4)
N2 C2 C1 115.5(4)
C3 C2 C1 122.9(4)
C4 C3 C2 120.3(4)
C3 C4 C5 119.4(4)
C6 C5 C4 118.3(5)
N2 C6 C5 122.0(4)
N1 C7 C8 110.5(4)
N3 C8 C9 120.4(7)
N3 C8 C7 116.2(4)
C9 C8 C7 123.5(5)
C10 C9 C8 120.1(6)
C9 C10 C11 119.5(5)
C10 C11 C12 118.8(7)
N3 C12 C11 122.0(6)
N1 C13 C14 110.3(3)
N4 C14 C13 110.5(3)
N4 C16 C17 111.7(3)
N5 C17 C18 121.7(4)
N5 C17 C16 116.9(3)
C18 C17 C16 121.4(3)
C19 C18 C17 119.1(4)
C18 C19 C20 119.5(4)
C19 C20 C21 118.2(4)
N5 C21 C20 123.3(4)
N2 Co1 N3 104.21(13)
N2 Co1 N4 144.32(13)
N3 Co1 N4 95.90(12)
N2 Co1 N1 75.29(14)
N3 Co1 N1 76.83(15)
N4 Co1 N1 81.15(13)
N2 Co1 N5 83.01(13)
N3 Co1 N5 171.64(13)
N4 Co1 N5 75.75(13)
N1 Co1 N5 101.36(13)
N2 Co1 Cl1 103.35(9)
N3 Co1 Cl1 93.32(10)
N4 Co1 Cl1 104.58(10)
N1 Co1 Cl1 169.19(10)
N5 Co1 Cl1 89.02(9)
C7 N1 C1 110.7(4)
C7 N1 C13 111.3(4)
C1 N1 C13 113.8(4)
C7 N1 Co1 106.7(3)
C1 N1 Co1 105.1(3)
C13 N1 Co1 108.8(3)
C2 N2 C6 118.6(4)
C2 N2 Co1 115.2(3)
C6 N2 Co1 124.5(3)
C12 N3 C8 119.2(4)
C12 N3 Co1 124.9(3)
C8 N3 Co1 115.2(3)
C15 N4 C16 108.7(3)
C15 N4 C14 111.5(4)
C16 N4 C14 108.6(3)
C15 N4 Co1 114.3(2)
C16 N4 Co1 107.1(2)
C14 N4 Co1 106.4(2)
C21 N5 C17 118.1(3)
C21 N5 Co1 129.8(3)
C17 N5 Co1 112.0(3)
F1 Sb1 F5 92.3(3)
F1 Sb1 F6 90.6(3)
F5 Sb1 F6 92.2(4)
F1 Sb1 F3 89.1(2)
F5 Sb1 F3 91.3(3)
F6 Sb1 F3 176.5(2)
F1 Sb1 F4 176.4(3)
F5 Sb1 F4 91.1(3)
F6 Sb1 F4 90.0(2)
F3 Sb1 F4 90.1(2)
F1 Sb1 F2 90.7(3)
F5 Sb1 F2 176.2(4)
F6 Sb1 F2 90.0(2)
F3 Sb1 F2 86.5(2)
F4 Sb1 F2 85.76(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.468(7)
C1 C2 1.494(7)
C2 N2 1.337(5)
C2 C3 1.382(7)
C3 C4 1.343(9)
C4 C5 1.393(8)
C5 C6 1.381(6)
C6 N2 1.354(5)
C7 N1 1.468(5)
C7 C8 1.468(9)
C8 N3 1.347(6)
C8 C9 1.387(7)
C9 C10 1.349(12)
C10 C11 1.366(13)
C11 C12 1.383(7)
C12 N3 1.327(6)
C13 N1 1.477(5)
C13 C14 1.512(6)
C14 N4 1.490(5)
C15 N4 1.462(6)
C16 N4 1.480(5)
C16 C17 1.483(6)
C17 N5 1.336(5)
C17 C18 1.396(5)
C18 C19 1.362(7)
C19 C20 1.374(7)
C20 C21 1.381(6)
C21 N5 1.330(6)
Cl1 Co1 2.3271(10)
Co1 N2 2.106(3)
Co1 N3 2.134(3)
Co1 N4 2.165(3)
Co1 N1 2.203(3)
Co1 N5 2.267(3)
F1 Sb1 1.822(4)
F2 Sb1 1.889(3)
F3 Sb1 1.856(3)
F4 Sb1 1.863(4)
F5 Sb1 1.827(4)
F6 Sb1 1.852(4)
