#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:16:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179405 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/02/4330233.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_4330233
loop_
_publ_author_name
'Julia Kozhukh'
'Stephen J. Lippard'
_publ_contact_author_address
;Department of Chemisry
Massachusetts Institute of Technology
Cambridge, MA 02139
;
_publ_contact_author_email       lippard@mit.edu
_publ_contact_author_name        'Stephen J. Lippard'
_publ_contact_author_phone       617-253-1892
_publ_section_title
;
 Variable Nitric Oxide Reactivity of Tropocoronand Cobalt(III) Nitrite
 Complexes as a Function of the Polymethylene Linker Chain Length
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9416
_journal_page_last               9422
_journal_paper_doi               10.1021/ic3012266
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C24 H30 Co N5 O2'
_chemical_formula_weight         479.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 90.910(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9717(17)
_cell_length_b                   13.0636(14)
_cell_length_c                   10.3826(11)
_cell_measurement_reflns_used    2692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.71
_cell_measurement_theta_min      2.55
_cell_volume                     2166.0(4)
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0728
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19369
_diffrn_reflns_theta_full        26.78
_diffrn_reflns_theta_max         26.78
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.9757
_exptl_absorpt_correction_T_min  0.8932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0385
_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)+(0.0238P)²+4.3776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                1844
_reflns_number_total             2319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3012266_si_003_2.cif
_cod_data_source_block           jk81_0m
_cod_database_code               4330233
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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 0.5000 0.22692(3) 0.2500 0.01312(13) Uani 1 2 d S
N1 N 0.45259(11) 0.22813(15) 0.07988(16) 0.0148(4) Uani 1 1 d .
O1 O 0.56303(10) 0.09415(13) 0.22533(14) 0.0201(4) Uani 1 1 d .
N3 N 0.5000 0.0383(2) 0.2500 0.0236(7) Uani 1 2 d S
C1 C 0.38840(14) 0.29131(17) 0.0602(2) 0.0158(5) Uani 1 1 d .
C7 C 0.36561(14) 0.34685(17) 0.1782(2) 0.0160(5) Uani 1 1 d .
C2 C 0.34989(15) 0.30693(18) -0.0627(2) 0.0196(5) Uani 1 1 d .
H2 H 0.3773 0.2734 -0.1314 0.023 Uiso 1 1 calc R
C4 C 0.22691(16) 0.42303(18) -0.0284(2) 0.0230(6) Uani 1 1 d .
H4 H 0.1805 0.4528 -0.0728 0.028 Uiso 1 1 calc R
C5 C 0.23549(15) 0.44447(18) 0.1016(2) 0.0214(5) Uani 1 1 d .
H5 H 0.1932 0.4874 0.1357 0.026 Uiso 1 1 calc R
C6 C 0.29643(15) 0.41289(18) 0.1902(2) 0.0202(5) Uani 1 1 d .
H6 H 0.2903 0.4409 0.2739 0.024 Uiso 1 1 calc R
C3 C 0.28012(15) 0.36181(18) -0.0999(2) 0.0212(5) Uani 1 1 d .
H3 H 0.2660 0.3571 -0.1889 0.025 Uiso 1 1 calc R
N2 N 0.41761(12) 0.32631(15) 0.27694(18) 0.0179(4) Uani 1 1 d .
C13 C 0.36634(17) 0.2389(2) 0.5377(3) 0.0361(7) Uani 1 1 d .
H13A H 0.3198 0.2212 0.5955 0.043 Uiso 1 1 calc R
H13B H 0.3611 0.1952 0.4602 0.043 Uiso 1 1 calc R
C11 C 0.41636(17) 0.3900(2) 0.3940(2) 0.0271(6) Uani 1 1 d .
H11A H 0.4002 0.4606 0.3695 0.033 Uiso 1 1 calc R
H11B H 0.4737 0.3928 0.4316 0.033 Uiso 1 1 calc R
C12 C 0.35664(19) 0.3517(2) 0.4965(3) 0.0372(7) Uani 1 1 d .
H12A H 0.2986 0.3618 0.4640 0.045 Uiso 1 1 calc R
H12B H 0.3640 0.3951 0.5740 0.045 Uiso 1 1 calc R
C15 C 0.51582(15) 0.16404(18) 0.5245(2) 0.0178(5) Uani 1 1 d .
H15A H 0.5634 0.1450 0.5819 0.021 Uiso 1 1 calc R
H15B H 0.4929 0.1001 0.4867 0.021 Uiso 1 1 calc R
C14 C 0.44790(17) 0.2143(2) 0.6056(2) 0.0307(6) Uani 1 1 d .
H14A H 0.4358 0.1684 0.6789 0.037 Uiso 1 1 calc R
H14B H 0.4710 0.2787 0.6419 0.037 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
N2 Co1 N2 92.22(12) 2_655 .
N2 Co1 N1 82.14(8) 2_655 2_655
N2 Co1 N1 97.19(8) . 2_655
N2 Co1 N1 97.19(8) 2_655 .
N2 Co1 N1 82.14(8) . .
N1 Co1 N1 179.05(12) 2_655 .
N2 Co1 O1 164.84(8) 2_655 2_655
N2 Co1 O1 102.89(8) . 2_655
N1 Co1 O1 94.63(7) 2_655 2_655
N1 Co1 O1 86.19(7) . 2_655
N2 Co1 O1 102.89(8) 2_655 .
N2 Co1 O1 164.84(8) . .
N1 Co1 O1 86.19(7) 2_655 .
N1 Co1 O1 94.63(7) . .
O1 Co1 O1 62.03(10) 2_655 .
C1 N1 C15 121.01(19) . 2_655
C1 N1 Co1 116.12(15) . .
C15 N1 Co1 122.87(15) 2_655 .
N3 O1 Co1 93.98(15) . .
O1 N3 O1 110.0(3) . 2_655
N1 C1 C2 123.2(2) . .
N1 C1 C7 112.2(2) . .
C2 C1 C7 124.5(2) . .
N2 C7 C6 122.3(2) . .
N2 C7 C1 112.3(2) . .
C6 C7 C1 125.4(2) . .
C3 C2 C1 131.6(2) . .
C5 C4 C3 125.8(2) . .
C4 C5 C6 130.0(2) . .
C5 C6 C7 131.7(2) . .
C2 C3 C4 130.5(2) . .
C7 N2 C11 120.2(2) . .
C7 N2 Co1 117.01(15) . .
C11 N2 Co1 122.24(15) . .
C14 C13 C12 114.6(3) . .
N2 C11 C12 114.0(2) . .
C11 C12 C13 116.5(2) . .
N1 C15 C14 114.6(2) 2_655 .
C13 C14 C15 116.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 1.8728(19) 2_655
Co1 N2 1.8728(19) .
Co1 N1 1.9107(18) 2_655
Co1 N1 1.9107(18) .
Co1 O1 2.0237(17) 2_655
Co1 O1 2.0237(17) .
N1 C1 1.329(3) .
N1 C15 1.465(3) 2_655
O1 N3 1.273(2) .
N3 O1 1.273(2) 2_655
C1 C2 1.423(3) .
C1 C7 1.474(3) .
C7 N2 1.336(3) .
C7 C6 1.409(3) .
C2 C3 1.375(3) .
C4 C5 1.384(3) .
C4 C3 1.390(3) .
C5 C6 1.391(3) .
N2 C11 1.473(3) .
C13 C14 1.506(4) .
C13 C12 1.542(4) .
C11 C12 1.524(4) .
C15 N1 1.465(3) 2_655
C15 C14 1.532(3) .
