#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:45:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179456 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/53/4335348.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_4335348
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                 101.421(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3825(10)
_cell_length_b                   14.1324(17)
_cell_length_c                   11.7395(15)
_cell_measurement_reflns_used    1624
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.66
_cell_measurement_theta_min      2.88
_cell_volume                     1525.8(3)
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_collection       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_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      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'APEX X8'
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9372
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0665
_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)+(0.0981P)²+2.4345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.1925
_reflns_number_gt                2499
_reflns_number_total             3483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400565h_si_001_1.cif
_cod_data_source_block           complex1123K
_cod_database_code               4335348
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 0.0192(2) Uani 1 2 d S
O1 O 0.4406(3) 0.6444(2) 0.4847(2) 0.0295(7) Uani 1 1 d .
O2 O 0.4440(3) 0.6867(2) 0.1937(3) 0.0387(7) Uani 1 1 d .
O3 O 1.0120(4) 0.8299(3) 0.5741(3) 0.0495(9) Uani 1 1 d .
O4 O 0.9772(5) 0.6836(3) 0.5295(5) 0.0769(14) Uani 1 1 d .
O5 O 0.7949(4) 0.7761(3) 0.5178(3) 0.0503(9) Uani 1 1 d .
N1 N 0.3619(3) 0.4771(2) 0.3541(3) 0.0227(7) Uani 1 1 d .
N2 N 0.6480(3) 0.5244(2) 0.4038(3) 0.0219(7) Uani 1 1 d .
N3 N 0.4312(4) 0.6806(2) 0.3822(3) 0.0311(8) Uani 1 1 d .
N4 N 0.9295(4) 0.7620(3) 0.5416(3) 0.0337(8) Uani 1 1 d .
C1 C 0.2748(4) 0.4012(3) 0.3363(4) 0.0284(9) Uani 1 1 d .
H1 H 0.2789 0.3576 0.3963 0.034 Uiso 1 1 calc R
C2 C 0.1794(4) 0.3851(3) 0.2327(4) 0.0312(9) Uani 1 1 d .
H2 H 0.1220 0.3309 0.2224 0.037 Uiso 1 1 calc R
C3 C 0.1703(4) 0.4504(3) 0.1450(4) 0.0367(11) Uani 1 1 d .
H3 H 0.1047 0.4418 0.0752 0.044 Uiso 1 1 calc R
C4 C 0.2588(5) 0.5286(3) 0.1610(4) 0.0336(10) Uani 1 1 d .
H4 H 0.2546 0.5731 0.1022 0.040 Uiso 1 1 calc R
C5 C 0.3541(4) 0.5400(3) 0.2658(4) 0.0259(8) Uani 1 1 d .
C6 C 0.4609(4) 0.6221(3) 0.2876(4) 0.0296(9) Uani 1 1 d .
C7 C 0.6158(4) 0.5849(3) 0.3139(3) 0.0247(8) Uani 1 1 d .
C8 C 0.7121(5) 0.6074(3) 0.2433(4) 0.0328(9) Uani 1 1 d .
H8 H 0.6874 0.6510 0.1833 0.039 Uiso 1 1 calc R
C9 C 0.8468(5) 0.5633(3) 0.2642(4) 0.0359(10) Uani 1 1 d .
H9 H 0.9141 0.5765 0.2179 0.043 Uiso 1 1 calc R
C10 C 0.8793(4) 0.4998(3) 0.3543(4) 0.0326(9) Uani 1 1 d .
H10 H 0.9684 0.4688 0.3685 0.039 Uiso 1 1 calc R
C11 C 0.7794(4) 0.4824(3) 0.4235(4) 0.0271(9) Uani 1 1 d .
H11 H 0.8033 0.4404 0.4854 0.033 Uiso 1 1 calc R
C12 C 0.3437(6) 0.7589(4) 0.2110(4) 0.0491(13) Uani 1 1 d .
H12A H 0.2449 0.7399 0.1777 0.059 Uiso 1 1 calc R
H12B H 0.3647 0.8174 0.1745 0.059 Uiso 1 1 calc R
C13 C 0.3623(4) 0.7723(3) 0.3440(4) 0.0304(9) Uani 1 1 d .
C14 C 0.2141(5) 0.7796(4) 0.3763(5) 0.0506(14) Uani 1 1 d .
H14A H 0.1504 0.7328 0.3343 0.076 Uiso 1 1 calc R
H14B H 0.1745 0.8415 0.3569 0.076 Uiso 1 1 calc R
H14C H 0.2236 0.7691 0.4583 0.076 Uiso 1 1 calc R
C15 C 0.4626(6) 0.8516(3) 0.3936(5) 0.0506(13) Uani 1 1 d .
H15A H 0.5544 0.8440 0.3702 0.076 Uiso 1 1 calc R
H15B H 0.4773 0.8503 0.4769 0.076 Uiso 1 1 calc R
H15C H 0.4202 0.9110 0.3655 0.076 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 180.000(1) . 3_666
N1 Co1 N2 93.01(13) . 3_666
N1 Co1 N2 86.99(13) 3_666 3_666
N1 Co1 N2 86.99(13) . .
N1 Co1 N2 93.01(13) 3_666 .
N2 Co1 N2 180.0 3_666 .
N1 Co1 O1 88.11(12) . .
N1 Co1 O1 91.89(12) 3_666 .
N2 Co1 O1 90.80(12) 3_666 .
N2 Co1 O1 89.20(12) . .
N1 Co1 O1 91.89(12) . 3_666
N1 Co1 O1 88.11(12) 3_666 3_666
N2 Co1 O1 89.20(12) 3_666 3_666
N2 Co1 O1 90.80(12) . 3_666
O1 Co1 O1 180.000(1) . 3_666
N3 O1 Co1 115.4(2) . .
C6 O2 C12 108.9(3) . .
C1 N1 C5 117.8(3) . .
C1 N1 Co1 123.1(3) . .
C5 N1 Co1 119.1(3) . .
C7 N2 C11 118.1(3) . .
C7 N2 Co1 118.9(2) . .
C11 N2 Co1 123.0(3) . .
O1 N3 C6 119.8(3) . .
O1 N3 C13 125.1(3) . .
C6 N3 C13 113.9(3) . .
O4 N4 O3 121.3(4) . .
O4 N4 O5 119.7(4) . .
O3 N4 O5 118.9(4) . .
N1 C1 C2 122.6(4) . .
N1 C1 H1 118.7 . .
C2 C1 H1 118.7 . .
C3 C2 C1 119.0(4) . .
C3 C2 H2 120.5 . .
C1 C2 H2 120.5 . .
C4 C3 C2 119.5(4) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
C3 C4 C5 119.0(4) . .
C3 C4 H4 120.5 . .
C5 C4 H4 120.5 . .
N1 C5 C4 122.2(4) . .
N1 C5 C6 115.9(3) . .
C4 C5 C6 121.9(4) . .
O2 C6 N3 102.6(3) . .
O2 C6 C7 109.6(3) . .
N3 C6 C7 111.2(3) . .
O2 C6 C5 113.1(3) . .
N3 C6 C5 110.1(3) . .
C7 C6 C5 110.0(3) . .
N2 C7 C8 123.1(4) . .
N2 C7 C6 115.9(3) . .
C8 C7 C6 120.9(4) . .
C7 C8 C9 118.2(4) . .
C7 C8 H8 120.9 . .
C9 C8 H8 120.9 . .
C10 C9 C8 119.0(4) . .
C10 C9 H9 120.5 . .
C8 C9 H9 120.5 . .
C9 C10 C11 119.8(4) . .
C9 C10 H10 120.1 . .
C11 C10 H10 120.1 . .
N2 C11 C10 121.7(4) . .
N2 C11 H11 119.1 . .
C10 C11 H11 119.1 . .
O2 C12 C13 106.6(4) . .
O2 C12 H12A 110.4 . .
C13 C12 H12A 110.4 . .
O2 C12 H12B 110.4 . .
C13 C12 H12B 110.4 . .
H12A C12 H12B 108.6 . .
N3 C13 C15 109.4(3) . .
N3 C13 C14 110.6(3) . .
C15 C13 C14 112.8(4) . .
N3 C13 C12 98.9(3) . .
C15 C13 C12 114.8(4) . .
C14 C13 C12 109.6(4) . .
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 1.959(3) .
Co1 N1 1.959(3) 3_666
Co1 N2 1.986(3) 3_666
Co1 N2 1.986(3) .
Co1 O1 2.113(3) .
Co1 O1 2.113(3) 3_666
O1 N3 1.294(4) .
O2 C6 1.416(5) .
O2 C12 1.429(6) .
O3 N4 1.244(5) .
O4 N4 1.215(5) .
O5 N4 1.254(5) .
N1 C1 1.340(5) .
N1 C5 1.356(5) .
N2 C7 1.346(5) .
N2 C11 1.347(5) .
N3 C6 1.455(5) .
N3 C13 1.478(5) .
C1 C2 1.379(6) .
C1 H1 0.9300 .
C2 C3 1.373(6) .
C2 H2 0.9300 .
C3 C4 1.372(6) .
C3 H3 0.9300 .
C4 C5 1.380(6) .
C4 H4 0.9300 .
C5 C6 1.521(6) .
C6 C7 1.518(5) .
C7 C8 1.379(6) .
C8 C9 1.386(6) .
C8 H8 0.9300 .
C9 C10 1.374(6) .
C9 H9 0.9300 .
C10 C11 1.380(6) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C12 C13 1.547(7) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C15 1.505(6) .
C13 C14 1.515(6) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
