#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/17/8101743.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_8101743
loop_
_publ_author_name
'Y.-L. Feng'
'H. Lin'
_publ_section_title
;
Crystal structure of bis(nitrito-N)(1,10-phenanthroline-N,N') (2,4-
pentanedionato-O,O')cobalt(III), Co(NO₂)₂(C₁₂H₈N₂)(C₅H₇O₂)
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              199
_journal_page_last               200
_journal_volume                  220
_journal_year                    2005
_chemical_formula_sum            'C17 H15 Co N4 O6'
_chemical_formula_weight         430.26
_chemical_name_systematic
; 
bis(nitrito-N)(1,10-phenanthroline-N,N')(2,4-pentanedionato-O,O')cobalt(III)
;
_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                 118.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.017(3)
_cell_length_b                   15.107(3)
_cell_length_c                   10.015(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1993.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       omega/phi
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2036
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.8404
_exptl_absorpt_correction_T_min  0.7739
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1337P)²+1.2102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1881
_reflns_number_gt                1053
_reflns_number_total             1378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1484.cff
_cod_data_source_block           d
_cod_original_cell_volume        1993.3(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               8101743
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.25124(5) 0.2500 0.0460(5) Uani 1 4 e d S . .
O1 O 0.4208(2) 0.1685(2) 0.1010(3) 0.0556(9) Uani 1 8 f d . . .
O2 O 0.5999(5) 0.1922(4) 0.0967(7) 0.141(3) Uani 1 8 f d . . .
O3 O 0.6683(3) 0.3058(3) 0.2243(6) 0.1001(15) Uani 1 8 f d . . .
N1 N 0.4307(3) 0.3470(3) 0.1090(4) 0.0510(10) Uani 1 8 f d . . .
N2 N 0.6014(4) 0.2496(3) 0.1808(5) 0.0549(12) Uani 1 8 f d . . .
C1 C 0.3650(5) 0.0325(4) -0.0237(7) 0.0748(17) Uani 1 8 f d . . .
H1A H 0.3229 0.0721 -0.1045 0.112 Uiso 1 8 f d R . .
H1B H 0.4066 -0.0015 -0.0537 0.112 Uiso 1 8 f d R . .
H1C H 0.3230 -0.0068 -0.0027 0.112 Uiso 1 8 f d R . .
C2 C 0.4314(4) 0.0845(3) 0.1163(6) 0.0536(12) Uani 1 8 f d . . .
C3 C 0.5000 0.0406(5) 0.2500 0.065(2) Uani 1 4 e d S . .
H3 H 0.5000 -0.0230 0.2500 0.078 Uiso 1 4 e d SR . .
C4 C 0.3584(4) 0.3428(4) -0.0361(5) 0.0604(13) Uani 1 8 f d . . .
H4 H 0.3351 0.2859 -0.0826 0.072 Uiso 1 8 f d R . .
C5 C 0.3162(4) 0.4181(4) -0.1211(6) 0.0730(16) Uani 1 8 f d . . .
H5 H 0.2652 0.4129 -0.2258 0.088 Uiso 1 8 f d R . .
C6 C 0.3459(5) 0.4992(4) -0.0586(7) 0.0740(16) Uani 1 8 f d . . .
H6 H 0.3150 0.5512 -0.1179 0.089 Uiso 1 8 f d R . .
C7 C 0.4635(4) 0.5892(4) 0.1761(7) 0.0782(17) Uani 1 8 f d . . .
H7 H 0.4381 0.6446 0.1247 0.094 Uiso 1 8 f d R . .
C8 C 0.4615(4) 0.4283(3) 0.1725(5) 0.0528(12) Uani 1 8 f d . . .
C9 C 0.4229(4) 0.5072(3) 0.0951(6) 0.0640(14) Uani 1 8 f d . . .
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
_geom_angle_publ_flag
O1 Co1 O1 96.2(2) . 2_655 ?
O1 Co1 N1 173.20(14) . 2_655 ?
O1 Co1 N1 90.22(17) 2_655 2_655 ?
O1 Co1 N1 90.22(17) . . ?
O1 Co1 N1 173.20(15) 2_655 . ?
N1 Co1 N1 83.5(2) 2_655 . ?
O1 Co1 N2 88.24(16) . 2_655 ?
O1 Co1 N2 90.79(17) 2_655 2_655 ?
N1 Co1 N2 89.34(16) 2_655 2_655 ?
N1 Co1 N2 91.74(18) . 2_655 ?
O1 Co1 N2 90.79(17) . . ?
O1 Co1 N2 88.24(16) 2_655 . ?
N1 Co1 N2 91.74(18) 2_655 . ?
N1 Co1 N2 89.34(16) . . ?
N2 Co1 N2 178.5(2) 2_655 . ?
C2 O1 Co1 124.9(3) . . ?
C4 N1 C8 118.0(4) . . ?
C4 N1 Co1 129.0(4) . . ?
C8 N1 Co1 113.0(3) . . ?
O2 N2 O3 119.0(5) . . ?
O2 N2 Co1 120.2(4) . . ?
O3 N2 Co1 120.7(4) . . ?
C2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.4 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 125.1(5) . . ?
O1 C2 C1 114.9(5) . . ?
C3 C2 C1 120.0(5) . . ?
C2 C3 C2 123.6(7) 2_655 . ?
C2 C3 H3 118.2 2_655 . ?
C2 C3 H3 118.2 . . ?
N1 C4 C5 121.7(5) . . ?
N1 C4 H4 119.2 . . ?
C5 C4 H4 119.1 . . ?
C6 C5 C4 120.7(5) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C9 119.7(5) . . ?
C5 C6 H6 120.2 . . ?
C9 C6 H6 120.1 . . ?
C7 C7 C9 121.0(3) 2_655 . ?
C7 C7 H7 119.4 2_655 . ?
C9 C7 H7 119.6 . . ?
N1 C8 C9 123.9(4) . . ?
N1 C8 C8 115.2(2) . 2_655 ?
C9 C8 C8 120.8(3) . 2_655 ?
C8 C9 C6 115.9(5) . . ?
C8 C9 C7 118.2(5) . . ?
C6 C9 C7 125.9(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 1.871(3) . ?
Co1 O1 1.871(3) 2_655 ?
Co1 N1 1.939(4) 2_655 ?
Co1 N1 1.939(4) . ?
Co1 N2 1.952(5) 2_655 ?
Co1 N2 1.952(5) . ?
O1 C2 1.279(6) . ?
O2 N2 1.203(6) . ?
O3 N2 1.224(6) . ?
N1 C4 1.335(6) . ?
N1 C8 1.359(6) . ?
C1 C2 1.495(7) . ?
C1 H1A 0.9601 . ?
C1 H1B 0.9601 . ?
C1 H1C 0.9600 . ?
C2 C3 1.404(6) . ?
C3 C2 1.404(6) 2_655 ?
C3 H3 0.9599 . ?
C4 C5 1.379(7) . ?
C4 H4 0.9600 . ?
C5 C6 1.350(9) . ?
C5 H5 0.9600 . ?
C6 C9 1.419(8) . ?
C6 H6 0.9600 . ?
C7 C7 1.355(12) 2_655 ?
C7 C9 1.445(8) . ?
C7 H7 0.9600 . ?
C8 C9 1.387(7) . ?
C8 C8 1.423(10) 2_655 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Co1 O1 C2 -1.9(3) 2_655 . . . ?
N1 Co1 O1 C2 -161.7(10) 2_655 . . . ?
N1 Co1 O1 C2 175.8(4) . . . . ?
N2 Co1 O1 C2 -92.5(4) 2_655 . . . ?
N2 Co1 O1 C2 86.4(4) . . . . ?
O1 Co1 N1 C4 -1.9(4) . . . . ?
O1 Co1 N1 C4 158.0(10) 2_655 . . . ?
N1 Co1 N1 C4 -179.2(5) 2_655 . . . ?
N2 Co1 N1 C4 -90.1(4) 2_655 . . . ?
N2 Co1 N1 C4 88.9(4) . . . . ?
O1 Co1 N1 C8 177.1(3) . . . . ?
O1 Co1 N1 C8 -23.0(13) 2_655 . . . ?
N1 Co1 N1 C8 -0.3(2) 2_655 . . . ?
N2 Co1 N1 C8 88.8(3) 2_655 . . . ?
N2 Co1 N1 C8 -92.1(3) . . . . ?
O1 Co1 N2 O2 -13.9(5) . . . . ?
O1 Co1 N2 O2 82.2(5) 2_655 . . . ?
N1 Co1 N2 O2 172.4(5) 2_655 . . . ?
N1 Co1 N2 O2 -104.1(5) . . . . ?
N2 Co1 N2 O2 34.1(5) 2_655 . . . ?
O1 Co1 N2 O3 167.4(4) . . . . ?
O1 Co1 N2 O3 -96.4(4) 2_655 . . . ?
N1 Co1 N2 O3 -6.3(4) 2_655 . . . ?
N1 Co1 N2 O3 77.2(4) . . . . ?
N2 Co1 N2 O3 -144.5(4) 2_655 . . . ?
Co1 O1 C2 C3 3.9(7) . . . . ?
Co1 O1 C2 C1 -174.8(3) . . . . ?
O1 C2 C3 C2 -2.2(4) . . . 2_655 ?
C1 C2 C3 C2 176.6(5) . . . 2_655 ?
C8 N1 C4 C5 0.7(7) . . . . ?
Co1 N1 C4 C5 179.6(4) . . . . ?
N1 C4 C5 C6 -1.1(8) . . . . ?
C4 C5 C6 C9 1.3(8) . . . . ?
C4 N1 C8 C9 -0.6(7) . . . . ?
Co1 N1 C8 C9 -179.7(4) . . . . ?
C4 N1 C8 C8 179.9(5) . . . 2_655 ?
Co1 N1 C8 C8 0.8(7) . . . 2_655 ?
N1 C8 C9 C6 0.8(7) . . . . ?
C8 C8 C9 C6 -179.7(5) 2_655 . . . ?
N1 C8 C9 C7 -179.2(5) . . . . ?
C8 C8 C9 C7 0.2(8) 2_655 . . . ?
C5 C6 C9 C8 -1.2(8) . . . . ?
C5 C6 C9 C7 178.9(5) . . . . ?
C7 C7 C9 C8 -0.6(10) 2_655 . . . ?
C7 C7 C9 C6 179.4(6) 2_655 . . . ?
