#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:16:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179405 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/02/4330232.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_4330232
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            'C22 H26 Co N5 O2'
_chemical_formula_weight         451.41
_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                 102.575(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.186(6)
_cell_length_b                   15.794(7)
_cell_length_c                   9.718(4)
_cell_measurement_reflns_used    2142
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.04
_cell_measurement_theta_min      2.58
_cell_volume                     1975.3(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0878
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16194
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.9564
_exptl_absorpt_correction_T_min  0.7148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0503
_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)+(0.0350P)²+3.8965P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                1523
_reflns_number_total             2022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3012266_si_003_1.cif
_cod_data_source_block           jk50_c2c
_cod_original_cell_volume        1975.1(15)
_cod_database_code               4330232
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 0.29804(4) 0.2500 0.0226(2) Uani 1 2 d S
N1 N 0.5472(2) 0.30311(19) 0.0784(3) 0.0254(6) Uani 1 1 d .
N2 N 0.3940(2) 0.37664(17) 0.1933(3) 0.0235(6) Uani 1 1 d .
C10 C 0.3698(3) 0.2873(2) -0.0729(4) 0.0329(8) Uani 1 1 d .
H10A H 0.3469 0.2561 0.0033 0.040 Uiso 1 1 calc R
H10B H 0.3333 0.2624 -0.1638 0.040 Uiso 1 1 calc R
C1 C 0.6390(3) 0.3403(2) 0.0882(4) 0.0250(7) Uani 1 1 d .
C7 C 0.6753(2) 0.3827(2) 0.2258(4) 0.0242(7) Uani 1 1 d .
C2 C 0.6934(3) 0.3408(2) -0.0217(4) 0.0288(8) Uani 1 1 d .
H2 H 0.6592 0.3115 -0.1041 0.035 Uiso 1 1 calc R
C8 C 0.3872(3) 0.4267(2) 0.0653(4) 0.0285(8) Uani 1 1 d .
H8A H 0.4581 0.4442 0.0585 0.034 Uiso 1 1 calc R
H8B H 0.3466 0.4786 0.0722 0.034 Uiso 1 1 calc R
C11 C 0.4854(3) 0.2736(2) -0.0572(4) 0.0335(9) Uani 1 1 d .
H11A H 0.4986 0.2124 -0.0672 0.040 Uiso 1 1 calc R
H11B H 0.5086 0.3037 -0.1342 0.040 Uiso 1 1 calc R
C4 C 0.8574(3) 0.4230(2) 0.0650(4) 0.0363(9) Uani 1 1 d .
H4 H 0.9179 0.4423 0.0363 0.044 Uiso 1 1 calc R
C6 C 0.7695(3) 0.4269(2) 0.2687(4) 0.0299(8) Uani 1 1 d .
H6 H 0.7812 0.4486 0.3620 0.036 Uiso 1 1 calc R
C3 C 0.7878(3) 0.3764(2) -0.0315(4) 0.0342(9) Uani 1 1 d .
H3 H 0.8075 0.3669 -0.1187 0.041 Uiso 1 1 calc R
C9 C 0.3367(3) 0.3789(2) -0.0685(4) 0.0332(9) Uani 1 1 d .
H9A H 0.2603 0.3807 -0.0788 0.040 Uiso 1 1 calc R
H9B H 0.3531 0.4089 -0.1504 0.040 Uiso 1 1 calc R
C5 C 0.8482(3) 0.4446(2) 0.1991(4) 0.0352(9) Uani 1 1 d .
H5 H 0.9045 0.4766 0.2520 0.042 Uiso 1 1 calc R
O1 O 0.42141(18) 0.18830(15) 0.2038(3) 0.0326(6) Uani 1 1 d .
N3 N 0.5000 0.1431(3) 0.2500 0.0346(10) 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'
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 96.31(17) 2_655 .
N2 Co1 N1 82.17(12) 2_655 .
N2 Co1 N1 94.60(12) . .
N2 Co1 N1 94.59(12) 2_655 2_655
N2 Co1 N1 82.17(12) . 2_655
N1 Co1 N1 175.18(18) . 2_655
N2 Co1 O1 162.65(11) 2_655 .
N2 Co1 O1 101.00(11) . .
N1 Co1 O1 95.22(11) . .
N1 Co1 O1 88.92(11) 2_655 .
N2 Co1 O1 101.00(11) 2_655 2_655
N2 Co1 O1 162.65(11) . 2_655
N1 Co1 O1 88.92(11) . 2_655
N1 Co1 O1 95.22(11) 2_655 2_655
O1 Co1 O1 61.73(14) . 2_655
N2 Co1 N3 131.84(8) 2_655 .
N2 Co1 N3 131.84(8) . .
N1 Co1 N3 92.41(9) . .
N1 Co1 N3 92.41(9) 2_655 .
O1 Co1 N3 30.86(7) . .
O1 Co1 N3 30.86(7) 2_655 .
C1 N1 C11 121.6(3) . .
C1 N1 Co1 114.9(2) . .
C11 N1 Co1 123.4(2) . .
C7 N2 C8 122.8(3) 2_655 .
C7 N2 Co1 116.1(2) 2_655 .
C8 N2 Co1 121.1(2) . .
C11 C10 C9 115.1(3) . .
N1 C1 C2 123.6(3) . .
N1 C1 C7 112.1(3) . .
C2 C1 C7 124.4(3) . .
N2 C7 C6 122.4(3) 2_655 .
N2 C7 C1 111.9(3) 2_655 .
C6 C7 C1 125.7(3) . .
C3 C2 C1 131.8(4) . .
N2 C8 C9 113.1(3) . .
N1 C11 C10 113.3(3) . .
C3 C4 C5 126.5(3) . .
C5 C6 C7 131.5(4) . .
C4 C3 C2 130.2(4) . .
C10 C9 C8 114.9(3) . .
C4 C5 C6 129.9(4) . .
N3 O1 Co1 93.7(2) . .
O1 N3 O1 110.8(4) . 2_655
O1 N3 Co1 55.4(2) . .
O1 N3 Co1 55.4(2) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 1.861(3) 2_655
Co1 N2 1.861(3) .
Co1 N1 1.904(3) .
Co1 N1 1.904(3) 2_655
Co1 O1 2.019(3) .
Co1 O1 2.019(3) 2_655
Co1 N3 2.447(5) .
N1 C1 1.331(4) .
N1 C11 1.466(4) .
N2 C7 1.333(4) 2_655
N2 C8 1.460(4) .
C10 C11 1.514(5) .
C10 C9 1.515(5) .
C1 C2 1.411(4) .
C1 C7 1.478(5) .
C7 N2 1.333(4) 2_655
C7 C6 1.407(5) .
C2 C3 1.388(5) .
C8 C9 1.525(5) .
C4 C3 1.375(5) .
C4 C5 1.379(5) .
C6 C5 1.384(5) .
O1 N3 1.258(3) .
N3 O1 1.258(3) 2_655
