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#$Date: 2019-11-24 11:30:18 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237801 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/87/4088737.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_4088737
loop_
_publ_author_name
'Hering, Florian'
'Berthel, Johannes H. J.'
'Lubitz, Katharina'
'Paul, Ursula S. D.'
'Schneider, Heidi'
'Härterich, Marcel'
'Radius, Udo'
_publ_section_title
;
 Synthesis and Thermal Properties of Novel NHC-Stabilized Cobalt Carbonyl
 Nitrosyl Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2806
_journal_paper_doi               10.1021/acs.organomet.6b00374
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C18.71 H32 Co N5.29 O2'
_chemical_formula_sum            'C18.71 H32 Co N5.29 O2'
_chemical_formula_weight         422.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3622(13)
_cell_length_b                   14.3857(15)
_cell_length_c                   16.751(2)
_cell_measurement_reflns_used    3811
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.083
_cell_measurement_theta_min      2.4315
_cell_volume                     2256.1(5)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_radiation_monochromator  helios
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15106
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.059
_diffrn_reflns_theta_min         2.432
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6766
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Sadabs 2014/4 (Bruker 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       bock
_exptl_crystal_F_000             897
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0394P)²+0.8435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1757
_reflns_number_total             2236
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00374_si_002.cif
_cod_data_source_block           compound_2
_cod_database_code               4088737
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.5000 0.51307(2) 0.7500 0.02850(13) Uani 1 2 d S T P . .
O4 O 0.46584(18) 0.62869(12) 0.88877(9) 0.0523(5) Uani 1 1 d . . . . .
N1 N 0.32100(17) 0.34878(10) 0.79894(9) 0.0302(4) Uani 1 1 d . . . . .
N2 N 0.25210(16) 0.39735(11) 0.68456(9) 0.0290(4) Uani 1 1 d . . . . .
C1 C 0.34666(19) 0.41697(12) 0.74436(10) 0.0245(4) Uani 1 1 d . . . . .
C2 C 0.1722(2) 0.31896(15) 0.70191(13) 0.0413(5) Uani 1 1 d . . . . .
H2 H 0.1005 0.2919 0.6692 0.050 Uiso 1 1 calc R U . . .
C3 C 0.2150(2) 0.28862(16) 0.77317(13) 0.0431(5) Uani 1 1 d . . . . .
H3 H 0.1797 0.2359 0.8010 0.052 Uiso 1 1 calc R U . . .
C4 C 0.2262(2) 0.45664(14) 0.61446(11) 0.0330(5) Uani 1 1 d . . . . .
H4 H 0.3153 0.4928 0.6036 0.040 Uiso 1 1 calc R U . . .
C5 C 0.3909(2) 0.34040(14) 0.87705(11) 0.0344(5) Uani 1 1 d . . . . .
H5 H 0.4623 0.3918 0.8821 0.041 Uiso 1 1 calc R U . . .
C6 C 0.1929(3) 0.39936(17) 0.54130(13) 0.0553(7) Uani 1 1 d . . . . .
H6A H 0.1870 0.4402 0.4946 0.083 Uiso 1 1 calc R U . . .
H6B H 0.1014 0.3674 0.5487 0.083 Uiso 1 1 calc R U . . .
H6C H 0.2687 0.3534 0.5331 0.083 Uiso 1 1 calc R U . . .
C7 C 0.1087(3) 0.5246(2) 0.63293(15) 0.0711(9) Uani 1 1 d . . . . .
H7A H 0.0926 0.5648 0.5866 0.107 Uiso 1 1 calc R U . . .
H7B H 0.1362 0.5627 0.6789 0.107 Uiso 1 1 calc R U . . .
H7C H 0.0208 0.4905 0.6453 0.107 Uiso 1 1 calc R U . . .
C8 C 0.4701(2) 0.24846(15) 0.88263(14) 0.0472(6) Uani 1 1 d . . . . .
H8A H 0.4020 0.1971 0.8774 0.071 Uiso 1 1 calc R U . . .
H8B H 0.5184 0.2443 0.9344 0.071 Uiso 1 1 calc R U . . .
H8C H 0.5410 0.2447 0.8397 0.071 Uiso 1 1 calc R U . . .
C9 C 0.2811(3) 0.35146(17) 0.94330(13) 0.0493(6) Uani 1 1 d . . . . .
H9A H 0.2308 0.4107 0.9367 0.074 Uiso 1 1 calc R U . . .
H9B H 0.3295 0.3506 0.9952 0.074 Uiso 1 1 calc R U . . .
H9C H 0.2123 0.3002 0.9407 0.074 Uiso 1 1 calc R U . . .
C10 C 0.48077(18) 0.57695(12) 0.83496(10) 0.0310(6) Uani 0.35(3) 1 d . . P A 1
N3 N 0.48077(18) 0.57695(12) 0.83496(10) 0.0310(6) Uani 0.65(3) 1 d . . P A 2
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
N3 Co N3 114.71(11) . 3_656
C10 Co C10 114.71(11) . 3_656
N3 Co C1 109.71(8) . .
C10 Co C1 109.71(8) . .
N3 Co C1 114.22(7) 3_656 .
C10 Co C1 114.22(7) 3_656 .
N3 Co C1 114.22(7) . 3_656
C10 Co C1 114.22(7) . 3_656
N3 Co C1 109.71(8) 3_656 3_656
C10 Co C1 109.71(8) 3_656 3_656
C1 Co C1 92.28(10) . 3_656
C1 N1 C3 111.52(16) . .
C1 N1 C5 125.36(16) . .
C3 N1 C5 123.08(16) . .
C1 N2 C2 111.38(16) . .
C1 N2 C4 124.91(15) . .
C2 N2 C4 123.42(16) . .
N1 C1 N2 103.24(15) . .
N1 C1 Co 126.44(13) . .
N2 C1 Co 130.10(13) . .
C3 C2 N2 107.00(18) . .
C3 C2 H2 126.5 . .
N2 C2 H2 126.5 . .
C2 C3 N1 106.85(18) . .
C2 C3 H3 126.6 . .
N1 C3 H3 126.6 . .
N2 C4 C7 109.46(17) . .
N2 C4 C6 111.44(17) . .
C7 C4 C6 111.78(19) . .
N2 C4 H4 108.0 . .
C7 C4 H4 108.0 . .
C6 C4 H4 108.0 . .
N1 C5 C8 110.12(17) . .
N1 C5 C9 109.90(17) . .
C8 C5 C9 112.08(17) . .
N1 C5 H5 108.2 . .
C8 C5 H5 108.2 . .
C9 C5 H5 108.2 . .
C4 C6 H6A 109.5 . .
C4 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C4 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C4 C7 H7A 109.5 . .
C4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C5 C9 H9A 109.5 . .
C5 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C5 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
O4 C10 Co 173.31(15) . .
O4 N3 Co 173.31(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N3 1.7036(18) .
Co C10 1.7036(18) .
Co N3 1.7036(18) 3_656
Co C10 1.7036(18) 3_656
Co C1 1.9953(18) .
Co C1 1.9953(18) 3_656
O4 N3 1.177(2) .
O4 C10 1.177(2) .
N1 C1 1.362(2) .
N1 C3 1.386(2) .
N1 C5 1.468(2) .
N2 C1 1.366(2) .
N2 C2 1.384(2) .
N2 C4 1.472(2) .
C2 C3 1.333(3) .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 C7 1.503(3) .
C4 C6 1.509(3) .
C4 H4 1.0000 .
C5 C8 1.519(3) .
C5 C9 1.521(3) .
C5 H5 1.0000 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
