#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:45:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179456 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/53/4335349.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_4335349
loop_
_publ_author_name
'Ian A. Gass'
'Subrata Tewary'
'Ayman Nafady'
'Nicholas F. Chilton'
'Christopher J. Gartshore'
'Mousa Asadi'
'David W. Lupton'
'Boujemaa Moubaraki'
'Alan M. Bond'
'John F. Boas'
'Si-Xuan Guo'
'Gopalan Rajaraman'
'Keith S. Murray'
_publ_contact_author_address
; School of Chemistry, 171 
  Monash university, 
  Vic 3800, 
  Australia
;
_publ_contact_author_email       Keith.murray@sci.monash.edu.au
_publ_contact_author_fax         +61-3-9905-4597
_publ_contact_author_name        'Keith. S. Murray'
_publ_contact_author_phone       +61-3-9905-4512
_publ_section_title
;
 Observation of Ferromagnetic Exchange, Spin Crossover, Reductively
 Induced Oxidation, and Field-Induced Slow Magnetic Relaxation in
 Monomeric Cobalt Nitroxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7557
_journal_page_last               7572
_journal_paper_doi               10.1021/ic400565h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
;
C30 H32 Co N6 O4, 2(N O3)
;
_chemical_formula_sum            'C30 H32 Co N8 O10'
_chemical_formula_weight         723.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '9 November 2005'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.495(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4583(5)
_cell_length_b                   14.0862(6)
_cell_length_c                   12.0890(6)
_cell_measurement_reflns_used    2469
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      32.2843
_cell_measurement_theta_min      2.1929
_cell_volume                     1578.33(14)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_measurement_method       'scans in phi and omega'
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8459
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0444
_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)+(0.0569P)²+0.9992P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                2827
_reflns_number_total             3623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400565h_si_001_2.cif
_cod_data_source_block           complex1273K
_cod_original_cell_volume        1578.33(13)
_cod_database_code               4335349
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.5000 0.5000 0.5000 0.02709(14) Uani 1 2 d S
O1 O 0.4412(2) 0.64504(12) 0.48260(13) 0.0372(4) Uani 1 1 d .
O2 O 0.4368(2) 0.68586(13) 0.19798(14) 0.0470(5) Uani 1 1 d .
O4 O 0.9865(4) 0.6838(2) 0.5358(4) 0.1230(14) Uani 1 1 d .
O3 O 1.0150(3) 0.83041(19) 0.5721(2) 0.0816(8) Uani 1 1 d .
O5 O 0.8042(3) 0.7745(2) 0.5195(3) 0.0950(10) Uani 1 1 d .
N1 N 0.3579(2) 0.47674(14) 0.35189(17) 0.0336(4) Uani 1 1 d .
N2 N 0.6483(2) 0.52581(14) 0.40020(17) 0.0325(4) Uani 1 1 d .
N3 N 0.4297(2) 0.67903(13) 0.38258(16) 0.0348(4) Uani 1 1 d .
N4 N 0.9363(3) 0.76150(17) 0.5424(2) 0.0514(6) Uani 1 1 d .
C1 C 0.2705(3) 0.40074(19) 0.3357(2) 0.0432(6) Uani 1 1 d .
H1 H 0.2736 0.3579 0.3946 0.052 Uiso 1 1 calc R
C2 C 0.1767(3) 0.3839(2) 0.2352(3) 0.0522(7) Uani 1 1 d .
H2 H 0.1190 0.3299 0.2262 0.063 Uiso 1 1 calc R
C3 C 0.1689(3) 0.4475(2) 0.1482(3) 0.0560(8) Uani 1 1 d .
H3 H 0.1048 0.4377 0.0802 0.067 Uiso 1 1 calc R
C4 C 0.2578(3) 0.5264(2) 0.1633(2) 0.0485(7) Uani 1 1 d .
H4 H 0.2545 0.5705 0.1056 0.058 Uiso 1 1 calc R
C5 C 0.3516(3) 0.53842(17) 0.2658(2) 0.0342(5) Uani 1 1 d .
C6 C 0.4584(3) 0.62121(16) 0.28746(19) 0.0347(5) Uani 1 1 d .
C7 C 0.6128(3) 0.58478(16) 0.3110(2) 0.0343(5) Uani 1 1 d .
C8 C 0.7065(3) 0.60723(19) 0.2407(2) 0.0455(6) Uani 1 1 d .
H8 H 0.6792 0.6489 0.1805 0.055 Uiso 1 1 calc R
C9 C 0.8423(3) 0.5659(2) 0.2623(3) 0.0534(7) Uani 1 1 d .
H9 H 0.9079 0.5794 0.2165 0.064 Uiso 1 1 calc R
C10 C 0.8792(3) 0.50467(19) 0.3521(3) 0.0481(7) Uani 1 1 d .
H10 H 0.9694 0.4757 0.3671 0.058 Uiso 1 1 calc R
C11 C 0.7804(3) 0.48689(17) 0.4193(2) 0.0399(6) Uani 1 1 d .
H11 H 0.8064 0.4462 0.4805 0.048 Uiso 1 1 calc R
C12 C 0.3579(6) 0.7636(2) 0.2214(3) 0.0886(15) Uani 1 1 d .
H12A H 0.2580 0.7565 0.1833 0.106 Uiso 1 1 calc R
H12B H 0.3956 0.8209 0.1933 0.106 Uiso 1 1 calc R
C13 C 0.3656(3) 0.77273(17) 0.3469(2) 0.0374(5) Uani 1 1 d .
C14 C 0.2179(4) 0.7805(3) 0.3756(4) 0.0866(13) Uani 1 1 d .
H14A H 0.1579 0.7298 0.3398 0.130 Uiso 1 1 calc R
H14B H 0.1754 0.8403 0.3494 0.130 Uiso 1 1 calc R
H14C H 0.2264 0.7763 0.4560 0.130 Uiso 1 1 calc R
C15 C 0.4635(5) 0.8497(2) 0.4034(4) 0.0789(11) Uani 1 1 d .
H15A H 0.5565 0.8434 0.3837 0.118 Uiso 1 1 calc R
H15B H 0.4735 0.8445 0.4838 0.118 Uiso 1 1 calc R
H15C H 0.4232 0.9105 0.3789 0.118 Uiso 1 1 calc R
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'
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 180.0 3_666 .
N1 Co1 N2 94.56(8) 3_666 .
N1 Co1 N2 85.44(8) . .
N1 Co1 N2 85.44(8) 3_666 3_666
N1 Co1 N2 94.56(8) . 3_666
N2 Co1 N2 180.0 . 3_666
N1 Co1 O1 87.35(7) 3_666 3_666
N1 Co1 O1 92.65(7) . 3_666
N2 Co1 O1 91.87(7) . 3_666
N2 Co1 O1 88.13(7) 3_666 3_666
N1 Co1 O1 92.65(7) 3_666 .
N1 Co1 O1 87.35(7) . .
N2 Co1 O1 88.13(7) . .
N2 Co1 O1 91.87(7) 3_666 .
O1 Co1 O1 180.0 3_666 .
N3 O1 Co1 115.13(13) . .
C12 O2 C6 111.0(2) . .
C1 N1 C5 118.0(2) . .
C1 N1 Co1 122.35(17) . .
C5 N1 Co1 119.63(16) . .
C11 N2 C7 117.6(2) . .
C11 N2 Co1 123.20(17) . .
C7 N2 Co1 119.18(16) . .
O1 N3 C6 122.18(18) . .
O1 N3 C13 124.02(19) . .
C6 N3 C13 113.14(17) . .
O4 N4 O3 120.9(3) . .
O4 N4 O5 120.9(3) . .
O3 N4 O5 118.2(3) . .
N1 C1 C2 122.5(3) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C3 C2 C1 119.5(3) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
C2 C3 C4 119.0(3) . .
C2 C3 H3 120.5 . .
C4 C3 H3 120.5 . .
C5 C4 C3 118.8(3) . .
C5 C4 H4 120.6 . .
C3 C4 H4 120.6 . .
N1 C5 C4 122.3(2) . .
N1 C5 C6 115.6(2) . .
C4 C5 C6 122.0(2) . .
O2 C6 N3 102.84(17) . .
O2 C6 C7 110.5(2) . .
N3 C6 C7 111.0(2) . .
O2 C6 C5 112.0(2) . .
N3 C6 C5 109.64(19) . .
C7 C6 C5 110.56(19) . .
N2 C7 C8 123.0(2) . .
N2 C7 C6 115.7(2) . .
C8 C7 C6 121.2(2) . .
C7 C8 C9 118.1(3) . .
C7 C8 H8 120.9 . .
C9 C8 H8 120.9 . .
C10 C9 C8 119.5(3) . .
C10 C9 H9 120.3 . .
C8 C9 H9 120.3 . .
C9 C10 C11 118.9(3) . .
C9 C10 H10 120.5 . .
C11 C10 H10 120.5 . .
N2 C11 C10 122.8(2) . .
N2 C11 H11 118.6 . .
C10 C11 H11 118.6 . .
O2 C12 C13 110.6(2) . .
O2 C12 H12A 109.5 . .
C13 C12 H12A 109.5 . .
O2 C12 H12B 109.5 . .
C13 C12 H12B 109.5 . .
H12A C12 H12B 108.1 . .
N3 C13 C15 109.4(2) . .
N3 C13 C14 110.0(2) . .
C15 C13 C14 111.1(3) . .
N3 C13 C12 98.7(2) . .
C15 C13 C12 114.9(3) . .
C14 C13 C12 112.1(3) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 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 2.040(2) 3_666
Co1 N1 2.040(2) .
Co1 N2 2.056(2) .
Co1 N2 2.056(2) 3_666
Co1 O1 2.1168(16) 3_666
Co1 O1 2.1168(16) .
O1 N3 1.285(2) .
O2 C12 1.387(4) .
O2 C6 1.397(3) .
O4 N4 1.202(4) .
O3 N4 1.232(3) .
O5 N4 1.238(3) .
N1 C1 1.343(3) .
N1 C5 1.348(3) .
N2 C11 1.342(3) .
N2 C7 1.350(3) .
N3 C6 1.478(3) .
N3 C13 1.480(3) .
C1 C2 1.375(4) .
C1 H1 0.9300 .
C2 C3 1.372(4) .
C2 H2 0.9300 .
C3 C4 1.384(4) .
C3 H3 0.9300 .
C4 C5 1.383(4) .
C4 H4 0.9300 .
C5 C6 1.531(3) .
C6 C7 1.520(3) .
C7 C8 1.381(3) .
C8 C9 1.387(4) .
C8 H8 0.9300 .
C9 C10 1.375(4) .
C9 H9 0.9300 .
C10 C11 1.378(4) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C12 C13 1.510(4) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C15 1.499(4) .
C13 C14 1.509(4) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
