#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:32:36 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178953 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/82/4118229.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_4118229
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
;
 Influence of Tetraazamacrocyclic Ligands on the Nitric Oxide Reactivity
 of their Cobalt(II) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11120
_journal_page_last               11123
_journal_paper_doi               10.1021/ja305011g
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C24 H30 Co N5 O'
_chemical_formula_weight         463.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.923(3)
_cell_angle_beta                 69.839(3)
_cell_angle_gamma                74.740(4)
_cell_formula_units_Z            2
_cell_length_a                   9.846(2)
_cell_length_b                   11.129(2)
_cell_length_c                   11.284(2)
_cell_measurement_reflns_used    7126
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.88
_cell_measurement_theta_min      2.23
_cell_volume                     1056.0(3)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18379
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.9513
_exptl_absorpt_correction_T_min  0.7299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0360
_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)+(0.0253P)²+0.8176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                4436
_reflns_number_total             5195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305011g_si_002_1.cif
_cod_data_source_block           jk56_0m
_cod_original_cell_volume        1056.0(4)
_cod_database_code               4118229
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.85080(3) 0.76743(2) 0.53046(2) 0.01287(7) Uani 1 1 d .
N4 N 0.86931(17) 0.89671(14) 0.35507(15) 0.0144(3) Uani 1 1 d .
N2 N 0.82021(17) 0.64355(14) 0.70856(15) 0.0145(3) Uani 1 1 d .
N1 N 0.83107(17) 0.61493(14) 0.49632(15) 0.0139(3) Uani 1 1 d .
N3 N 0.70580(16) 0.90758(14) 0.57557(15) 0.0139(3) Uani 1 1 d .
N5 N 1.02608(18) 0.78770(15) 0.52741(16) 0.0180(3) Uani 1 1 d .
O1 O 1.10712(16) 0.85929(14) 0.44413(14) 0.0260(3) Uani 1 1 d .
C6 C 0.6929(2) 0.46101(18) 0.86365(18) 0.0190(4) Uani 1 1 d .
H6 H 0.7017 0.4851 0.9323 0.023 Uiso 1 1 calc R
C13 C 0.6977(2) 1.02341(17) 0.47754(18) 0.0145(4) Uani 1 1 d .
C1 C 0.75844(19) 0.52778(17) 0.60625(17) 0.0141(4) Uani 1 1 d .
C2 C 0.7006(2) 0.42696(17) 0.60118(18) 0.0169(4) Uani 1 1 d .
H2 H 0.7142 0.4284 0.5131 0.020 Uiso 1 1 calc R
C9 C 0.7900(2) 0.72609(18) 0.90198(18) 0.0198(4) Uani 1 1 d .
H9A H 0.8356 0.7022 0.9754 0.024 Uiso 1 1 calc R
H9B H 0.6907 0.7007 0.9429 0.024 Uiso 1 1 calc R
C7 C 0.7528(2) 0.54462(17) 0.73162(18) 0.0146(4) Uani 1 1 d .
C8 C 0.8797(2) 0.64484(18) 0.81068(18) 0.0178(4) Uani 1 1 d .
H8A H 0.9755 0.6768 0.7642 0.021 Uiso 1 1 calc R
H8B H 0.8991 0.5523 0.8687 0.021 Uiso 1 1 calc R
C14 C 0.5951(2) 1.13512(18) 0.49573(19) 0.0183(4) Uani 1 1 d .
H14 H 0.5260 1.1182 0.5813 0.022 Uiso 1 1 calc R
C12 C 0.5976(2) 0.88883(18) 0.70677(18) 0.0156(4) Uani 1 1 d .
H12A H 0.5923 0.7933 0.7525 0.019 Uiso 1 1 calc R
H12B H 0.5004 0.9332 0.6928 0.019 Uiso 1 1 calc R
C11 C 0.6310(2) 0.94196(18) 0.79792(19) 0.0199(4) Uani 1 1 d .
H11A H 0.6331 1.0381 0.7534 0.024 Uiso 1 1 calc R
H11B H 0.5506 0.9294 0.8817 0.024 Uiso 1 1 calc R
C10 C 0.7749(2) 0.87716(19) 0.83337(19) 0.0208(4) Uani 1 1 d .
H10A H 0.7863 0.9170 0.8933 0.025 Uiso 1 1 calc R
H10B H 0.8560 0.8977 0.7503 0.025 Uiso 1 1 calc R
C3 C 0.6275(2) 0.32624(18) 0.70139(19) 0.0195(4) Uani 1 1 d .
H3 H 0.5959 0.2735 0.6701 0.023 Uiso 1 1 calc R
C4 C 0.5930(2) 0.28958(19) 0.8396(2) 0.0232(4) Uani 1 1 d .
H4 H 0.5432 0.2152 0.8905 0.028 Uiso 1 1 calc R
C5 C 0.6246(2) 0.3519(2) 0.9101(2) 0.0233(4) Uani 1 1 d .
H5 H 0.5945 0.3132 1.0047 0.028 Uiso 1 1 calc R
C19 C 0.8010(2) 1.01833(17) 0.34832(18) 0.0148(4) Uani 1 1 d .
C23 C 0.7808(2) 0.64119(18) 0.27912(18) 0.0189(4) Uani 1 1 d .
H23A H 0.8227 0.6048 0.2046 0.023 Uiso 1 1 calc R
H23B H 0.6852 0.6099 0.3304 0.023 Uiso 1 1 calc R
C24 C 0.8824(2) 0.58431(17) 0.37108(18) 0.0159(4) Uani 1 1 d .
H24A H 0.9006 0.4871 0.3943 0.019 Uiso 1 1 calc R
H24B H 0.9773 0.6167 0.3198 0.019 Uiso 1 1 calc R
C21 C 0.8909(2) 0.85835(19) 0.14567(18) 0.0210(4) Uani 1 1 d .
H21A H 0.8632 0.9483 0.0865 0.025 Uiso 1 1 calc R
H21B H 0.9602 0.8083 0.0878 0.025 Uiso 1 1 calc R
C18 C 0.8261(2) 1.12913(18) 0.22892(19) 0.0198(4) Uani 1 1 d .
H18 H 0.8969 1.1088 0.1546 0.024 Uiso 1 1 calc R
C15 C 0.5769(2) 1.26418(19) 0.4119(2) 0.0216(4) Uani 1 1 d .
H15 H 0.4989 1.3208 0.4501 0.026 Uiso 1 1 calc R
C22 C 0.7537(2) 0.79164(18) 0.21954(18) 0.0179(4) Uani 1 1 d .
H22A H 0.6956 0.8274 0.2928 0.022 Uiso 1 1 calc R
H22B H 0.6938 0.8162 0.1565 0.022 Uiso 1 1 calc R
C20 C 0.9708(2) 0.86949(18) 0.23602(18) 0.0176(4) Uani 1 1 d .
H20A H 1.0369 0.7859 0.2638 0.021 Uiso 1 1 calc R
H20B H 1.0316 0.9411 0.1843 0.021 Uiso 1 1 calc R
C16 C 0.6537(2) 1.32491(19) 0.2811(2) 0.0249(4) Uani 1 1 d .
H16 H 0.6276 1.4175 0.2429 0.030 Uiso 1 1 calc R
C17 C 0.7660(2) 1.26123(19) 0.2013(2) 0.0224(4) Uani 1 1 d .
H17 H 0.8081 1.3172 0.1142 0.027 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
N5 Co1 N2 92.50(7)
N5 Co1 N4 90.03(7)
N2 Co1 N4 176.48(7)
N5 Co1 N3 109.83(7)
N2 Co1 N3 96.12(6)
N4 Co1 N3 80.71(6)
N5 Co1 N1 119.70(7)
N2 Co1 N1 80.65(6)
N4 Co1 N1 100.20(6)
N3 Co1 N1 130.44(7)
C19 N4 C20 120.66(15)
C19 N4 Co1 116.75(12)
C20 N4 Co1 121.94(11)
C7 N2 C8 120.34(15)
C7 N2 Co1 115.03(12)
C8 N2 Co1 124.26(12)
C1 N1 C24 117.53(15)
C1 N1 Co1 112.69(12)
C24 N1 Co1 129.78(12)
C13 N3 C12 119.83(15)
C13 N3 Co1 116.84(12)
C12 N3 Co1 123.08(11)
O1 N5 Co1 129.48(13)
C5 C6 C7 131.93(18)
N3 C13 C14 123.09(17)
N3 C13 C19 112.25(15)
C14 C13 C19 124.56(16)
N1 C1 C2 122.83(16)
N1 C1 C7 112.89(16)
C2 C1 C7 124.20(16)
C3 C2 C1 131.70(18)
C8 C9 C10 115.49(16)
N2 C7 C6 122.14(17)
N2 C7 C1 112.09(16)
C6 C7 C1 125.63(17)
N2 C8 C9 119.03(16)
C15 C14 C13 131.80(19)
N3 C12 C11 114.09(16)
C10 C11 C12 114.39(15)
C11 C10 C9 115.07(17)
C4 C3 C2 130.88(19)
C3 C4 C5 125.82(19)
C6 C5 C4 129.78(19)
N4 C19 C18 122.98(17)
N4 C19 C13 112.12(15)
C18 C19 C13 124.90(16)
C22 C23 C24 115.79(16)
N1 C24 C23 116.76(15)
C22 C21 C20 115.31(15)
C17 C18 C19 131.68(19)
C14 C15 C16 130.69(19)
C23 C22 C21 115.57(16)
N4 C20 C21 112.22(16)
C15 C16 C17 125.29(18)
C18 C17 C16 130.25(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 N5 1.7856(17)
Co1 N2 1.9129(15)
Co1 N4 1.9176(15)
Co1 N3 1.9183(15)
Co1 N1 1.9504(16)
N4 C19 1.329(2)
N4 C20 1.459(2)
N2 C7 1.327(2)
N2 C8 1.468(2)
N1 C1 1.342(2)
N1 C24 1.471(2)
N3 C13 1.334(2)
N3 C12 1.469(2)
N5 O1 1.177(2)
C6 C5 1.375(3)
C6 C7 1.425(2)
C13 C14 1.416(2)
C13 C19 1.475(3)
C1 C2 1.413(3)
C1 C7 1.479(2)
C2 C3 1.387(3)
C9 C8 1.530(3)
C9 C10 1.541(3)
C14 C15 1.381(3)
C12 C11 1.526(3)
C11 C10 1.521(3)
C3 C4 1.386(3)
C4 C5 1.388(3)
C19 C18 1.423(2)
C23 C22 1.527(3)
C23 C24 1.531(3)
C21 C22 1.529(3)
C21 C20 1.542(3)
C18 C17 1.385(3)
C15 C16 1.387(3)
C16 C17 1.391(3)
