#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:34:58 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179252 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/72/4317221.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_4317221
loop_
_publ_author_name
'Jeremy M. Smith'
'Jeffrey R. Long'
_publ_section_title
;
 First-Row Transition Metal Complexes of the Strongly Donating
 Pentadentate Ligand PY4Im
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11223
_journal_page_last               11230
_journal_paper_doi               10.1021/ic1018407
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C29 H23 Co F6 N7 O6 S2'
_chemical_formula_weight         802.59
_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
_audit_update_record
;
2010-08-06 # Formatted by publCIF
;
_cell_angle_alpha                97.247(5)
_cell_angle_beta                 96.493(5)
_cell_angle_gamma                116.668(5)
_cell_formula_units_Z            2
_cell_length_a                   10.700(5)
_cell_length_b                   11.756(5)
_cell_length_c                   15.505(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1697.0(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21581
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.637
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1874P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2305
_refine_ls_wR_factor_ref         0.2710
_reflns_number_gt                4084
_reflns_number_total             6177
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic1018407_si_002_4.cif
_cod_data_source_block           jms3a
_cod_database_code               4317221
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.01846(7) 0.37954(7) 0.73846(4) 0.0239(3) Uani 1 1 d . . .
S1 S 0.31538(15) 0.22325(15) 0.48604(10) 0.0316(4) Uani 1 1 d . . .
S2 S 0.3117(2) 1.02125(19) 0.97038(12) 0.0505(5) Uani 1 1 d . . .
O1 O 0.2444(5) 0.2285(5) 0.4035(3) 0.0476(12) Uani 1 1 d . . .
O3 O 0.4572(5) 0.3267(4) 0.5168(3) 0.0448(12) Uani 1 1 d . . .
N21 N 0.0745(5) 0.6392(4) 0.7963(3) 0.0266(11) Uani 1 1 d . . .
O2 O 0.2320(5) 0.1918(5) 0.5535(3) 0.0548(13) Uani 1 1 d . . .
N11 N -0.1244(5) 0.5280(5) 0.7062(3) 0.0290(11) Uani 1 1 d . . .
F2 F 0.2159(5) -0.0255(4) 0.4251(3) 0.0767(15) Uani 1 1 d . . .
F3 F 0.3981(6) 0.0560(5) 0.5296(3) 0.0702(14) Uani 1 1 d . . .
O4 O 0.2966(5) 0.9761(4) 0.8776(3) 0.0474(12) Uani 1 1 d . . .
N13 N -0.0610(5) 0.3440(4) 0.6053(3) 0.0268(11) Uani 1 1 d . . .
N12 N 0.2425(5) 0.5166(5) 0.7365(3) 0.0293(11) Uani 1 1 d . . .
N14 N 0.0931(5) 0.4360(5) 0.8742(3) 0.0289(11) Uani 1 1 d . . .
C55 C -0.3014(6) 0.3065(6) 0.7041(3) 0.0286(13) Uani 1 1 d . . .
F1 F 0.4241(6) 0.0924(5) 0.3994(3) 0.0745(14) Uani 1 1 d . . .
C31 C 0.0166(7) 0.7217(6) 0.7871(4) 0.0316(14) Uani 1 1 d . . .
H35 H 0.0565 0.8087 0.8142 0.038 Uiso 1 1 calc R . .
C2 C -0.2375(6) 0.4094(5) 0.6488(3) 0.0277(13) Uani 1 1 d . . .
H2 H -0.3117 0.4274 0.6208 0.033 Uiso 1 1 calc R . .
N15 N -0.2128(5) 0.2663(5) 0.7429(3) 0.0325(12) Uani 1 1 d . . .
C12 C 0.2993(6) 0.6342(6) 0.7879(4) 0.0284(13) Uani 1 1 d . . .
N16 N 0.0489(5) 0.2264(5) 0.7269(3) 0.0295(11) Uani 1 1 d . . .
C1 C 0.2099(6) 0.6576(5) 0.8487(4) 0.0316(14) Uani 1 1 d . . .
H1 H 0.2626 0.7467 0.8832 0.038 Uiso 1 1 calc R . .
C53 C -0.1739(6) 0.3637(5) 0.5778(4) 0.0269(13) Uani 1 1 d . . .
C11 C -0.0118(5) 0.5229(5) 0.7479(4) 0.0255(12) Uani 1 1 d . . .
C21 C -0.1101(6) 0.6505(6) 0.7304(4) 0.0307(13) Uani 1 1 d . . .
H25 H -0.1748 0.6790 0.7115 0.037 Uiso 1 1 calc R . .
C3 C 0.3400(7) 0.0797(7) 0.4586(4) 0.0426(16) Uani 1 1 d . . .
C44 C 0.2298(7) 0.6098(7) 1.0012(4) 0.0411(16) Uani 1 1 d . . .
H22 H 0.2869 0.6978 1.0249 0.049 Uiso 1 1 calc R . .
C13 C -0.0069(6) 0.3010(6) 0.5431(4) 0.0323(14) Uani 1 1 d . . .
H53 H 0.0696 0.2863 0.5610 0.039 Uiso 1 1 calc R . .
C54 C 0.1750(6) 0.5639(6) 0.9109(3) 0.0274(13) Uani 1 1 d . . .
C26 C 0.0831(7) 0.0231(6) 0.6940(5) 0.0411(16) Uani 1 1 d . . .
H26A H -0.0082 -0.0510 0.6704 0.062 Uiso 1 1 calc R . .
H26B H 0.1255 0.0100 0.7472 0.062 Uiso 1 1 calc R . .
H26C H 0.1436 0.0341 0.6511 0.062 Uiso 1 1 calc R . .
C22 C 0.4351(7) 0.7296(6) 0.7877(4) 0.0398(16) Uani 1 1 d . . .
H21 H 0.4718 0.8115 0.8236 0.048 Uiso 1 1 calc R . .
C23 C -0.0584(7) 0.2776(6) 0.4545(4) 0.0417(16) Uani 1 1 d . . .
H43 H -0.0158 0.2493 0.4138 0.050 Uiso 1 1 calc R . .
C45 C -0.4427(7) 0.2593(7) 0.7124(4) 0.0465(18) Uani 1 1 d . . .
H24 H -0.5009 0.2872 0.6827 0.056 Uiso 1 1 calc R . .
C43 C -0.2335(6) 0.3388(6) 0.4890(4) 0.0350(14) Uani 1 1 d . . .
H23 H -0.3124 0.3504 0.4718 0.042 Uiso 1 1 calc R . .
O6 O 0.2340(8) 0.9209(7) 1.0169(4) 0.092(2) Uani 1 1 d . . .
F6 F 0.2157(8) 1.1640(8) 1.0534(5) 0.129(3) Uani 1 1 d . . .
C24 C 0.1143(8) 0.3875(7) 1.0178(4) 0.0442(17) Uani 1 1 d . . .
H42 H 0.0927 0.3247 1.0526 0.053 Uiso 1 1 calc R . .
O5 O 0.4517(7) 1.1130(8) 1.0131(5) 0.104(3) Uani 1 1 d . . .
C15 C -0.2682(7) 0.1759(6) 0.7914(4) 0.0386(15) Uani 1 1 d . . .
H54 H -0.2098 0.1456 0.8178 0.046 Uiso 1 1 calc R . .
C32 C 0.5167(7) 0.7007(8) 0.7324(5) 0.0490(19) Uani 1 1 d . . .
H31 H 0.6088 0.7629 0.7316 0.059 Uiso 1 1 calc R . .
C25 C -0.4057(8) 0.1252(7) 0.8046(4) 0.0489(19) Uani 1 1 d . . .
H44 H -0.4388 0.0621 0.8389 0.059 Uiso 1 1 calc R . .
C42 C 0.4594(7) 0.5809(7) 0.6801(5) 0.0418(16) Uani 1 1 d . . .
H41 H 0.5103 0.5597 0.6420 0.050 Uiso 1 1 calc R . .
C52 C 0.3224(7) 0.4907(7) 0.6854(4) 0.0390(15) Uani 1 1 d . . .
H51 H 0.2843 0.4075 0.6513 0.047 Uiso 1 1 calc R . .
C14 C 0.0662(7) 0.3518(6) 0.9291(4) 0.0358(15) Uani 1 1 d . . .
H52 H 0.0113 0.2638 0.9047 0.043 Uiso 1 1 calc R . .
C33 C -0.1723(7) 0.2957(7) 0.4257(4) 0.0458(18) Uani 1 1 d . . .
H33 H -0.2085 0.2798 0.3655 0.055 Uiso 1 1 calc R . .
C34 C 0.1937(9) 0.5148(9) 1.0554(4) 0.052(2) Uani 1 1 d . . .
H32 H 0.2247 0.5402 1.1165 0.063 Uiso 1 1 calc R . .
F4 F 0.0835(8) 1.0442(9) 0.9275(5) 0.136(3) Uani 1 1 d . . .
C16 C 0.0652(6) 0.1388(6) 0.7139(4) 0.0326(14) Uani 1 1 d . . .
F5 F 0.2668(9) 1.2079(7) 0.9254(5) 0.136(3) Uani 1 1 d . . .
C35 C -0.4950(7) 0.1689(8) 0.7663(5) 0.061(2) Uani 1 1 d . . .
H34 H -0.5876 0.1387 0.7764 0.073 Uiso 1 1 calc R . .
C4 C 0.2178(12) 1.1169(11) 0.9701(7) 0.083(3) Uani 1 1 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C11 Co1 N16 179.3(2) . . ?
C11 Co1 N13 86.4(2) . . ?
N16 Co1 N13 92.85(19) . . ?
C11 Co1 N14 86.0(2) . . ?
N16 Co1 N14 94.69(19) . . ?
N13 Co1 N14 172.46(19) . . ?
C11 Co1 N12 85.9(2) . . ?
N16 Co1 N12 94.43(19) . . ?
N13 Co1 N12 97.71(17) . . ?
N14 Co1 N12 82.03(18) . . ?
C11 Co1 N15 85.8(2) . . ?
N16 Co1 N15 93.85(19) . . ?
N13 Co1 N15 82.11(17) . . ?
N14 Co1 N15 97.07(18) . . ?
N12 Co1 N15 171.71(18) . . ?
O2 S1 O3 114.2(3) . . ?
O2 S1 O1 115.8(3) . . ?
O3 S1 O1 114.8(3) . . ?
O2 S1 C3 102.4(3) . . ?
O3 S1 C3 103.8(3) . . ?
O1 S1 C3 103.5(3) . . ?
O5 S2 O4 114.4(4) . . ?
O5 S2 O6 116.4(5) . . ?
O4 S2 O6 114.3(4) . . ?
O5 S2 C4 103.1(5) . . ?
O4 S2 C4 102.1(4) . . ?
O6 S2 C4 103.9(5) . . ?
C11 N21 C31 110.1(5) . . ?
C11 N21 C1 117.2(5) . . ?
C31 N21 C1 132.6(5) . . ?
C11 N11 C21 109.5(5) . . ?
C11 N11 C2 118.0(5) . . ?
C21 N11 C2 132.5(5) . . ?
C13 N13 C53 117.6(5) . . ?
C13 N13 Co1 122.7(4) . . ?
C53 N13 Co1 119.7(4) . . ?
C12 N12 C52 118.0(5) . . ?
C12 N12 Co1 117.6(4) . . ?
C52 N12 Co1 124.4(4) . . ?
C14 N14 C54 117.0(5) . . ?
C14 N14 Co1 123.3(4) . . ?
C54 N14 Co1 119.6(3) . . ?
N15 C55 C45 123.7(5) . . ?
N15 C55 C2 116.1(5) . . ?
C45 C55 C2 120.2(5) . . ?
C21 C31 N21 106.2(5) . . ?
N11 C2 C53 108.5(4) . . ?
N11 C2 C55 109.2(4) . . ?
C53 C2 C55 110.6(5) . . ?
C15 N15 C55 116.4(5) . . ?
C15 N15 Co1 125.8(4) . . ?
C55 N15 Co1 116.9(4) . . ?
N12 C12 C22 122.3(6) . . ?
N12 C12 C1 116.6(5) . . ?
C22 C12 C1 121.0(6) . . ?
C16 N16 Co1 175.0(5) . . ?
N21 C1 C12 110.0(5) . . ?
N21 C1 C54 108.8(4) . . ?
C12 C1 C54 110.2(5) . . ?
N13 C53 C43 122.1(5) . . ?
N13 C53 C2 117.4(5) . . ?
C43 C53 C2 120.4(5) . . ?
N21 C11 N11 107.4(5) . . ?
N21 C11 Co1 126.4(4) . . ?
N11 C11 Co1 126.2(4) . . ?
C31 C21 N11 106.7(5) . . ?
F3 C3 F2 107.1(6) . . ?
F3 C3 F1 107.2(6) . . ?
F2 C3 F1 107.5(6) . . ?
F3 C3 S1 111.5(5) . . ?
F2 C3 S1 111.1(5) . . ?
F1 C3 S1 112.3(5) . . ?
C54 C44 C34 116.4(6) . . ?
N13 C13 C23 123.2(6) . . ?
N14 C54 C44 123.2(5) . . ?
N14 C54 C1 116.9(5) . . ?
C44 C54 C1 119.9(5) . . ?
C12 C22 C32 118.7(6) . . ?
C13 C23 C33 120.1(6) . . ?
C55 C45 C35 118.1(7) . . ?
C53 C43 C33 118.6(6) . . ?
C34 C24 C14 119.6(6) . . ?
N15 C15 C25 124.0(6) . . ?
C42 C32 C22 119.2(6) . . ?
C15 C25 C35 119.2(6) . . ?
C32 C42 C52 118.0(7) . . ?
N12 C52 C42 123.7(6) . . ?
N14 C14 C24 123.9(6) . . ?
C23 C33 C43 118.3(6) . . ?
C24 C34 C44 119.7(6) . . ?
N16 C16 C26 178.0(6) . . ?
C25 C35 C45 118.3(7) . . ?
F5 C4 F4 102.7(9) . . ?
F5 C4 F6 111.6(9) . . ?
F4 C4 F6 107.9(9) . . ?
F5 C4 S2 113.1(8) . . ?
F4 C4 S2 110.4(8) . . ?
F6 C4 S2 110.7(7) . . ?
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 C11 1.845(6) . ?
Co1 N16 1.958(5) . ?
Co1 N13 2.056(5) . ?
Co1 N14 2.073(5) . ?
Co1 N12 2.214(5) . ?
Co1 N15 2.238(5) . ?
S1 O2 1.428(5) . ?
S1 O3 1.429(4) . ?
S1 O1 1.436(4) . ?
S1 C3 1.828(7) . ?
S2 O5 1.411(7) . ?
S2 O4 1.433(5) . ?
S2 O6 1.440(6) . ?
S2 C4 1.813(10) . ?
N21 C11 1.317(7) . ?
N21 C31 1.378(8) . ?
N21 C1 1.487(7) . ?
N11 C11 1.331(7) . ?
N11 C21 1.374(8) . ?
N11 C2 1.460(7) . ?
F2 C3 1.330(8) . ?
F3 C3 1.325(7) . ?
N13 C13 1.337(8) . ?
N13 C53 1.361(7) . ?
N12 C12 1.331(8) . ?
N12 C52 1.335(8) . ?
N14 C14 1.341(7) . ?
N14 C54 1.357(7) . ?
C55 N15 1.352(7) . ?
C55 C45 1.385(8) . ?
C55 C2 1.522(7) . ?
F1 C3 1.332(8) . ?
C31 C21 1.356(8) . ?
C2 C53 1.521(8) . ?
N15 C15 1.335(7) . ?
C12 C22 1.381(8) . ?
C12 C1 1.503(9) . ?
N16 C16 1.118(8) . ?
C1 C54 1.504(8) . ?
C53 C43 1.386(8) . ?
C44 C54 1.391(8) . ?
C44 C34 1.423(9) . ?
C13 C23 1.364(8) . ?
C26 C16 1.457(9) . ?
C22 C32 1.406(10) . ?
C23 C33 1.366(10) . ?
C45 C35 1.392(9) . ?
C43 C33 1.403(9) . ?
F6 C4 1.347(12) . ?
C24 C34 1.353(11) . ?
C24 C14 1.354(9) . ?
C15 C25 1.369(10) . ?
C32 C42 1.357(10) . ?
C25 C35 1.386(11) . ?
C42 C52 1.391(9) . ?
F4 C4 1.331(12) . ?
F5 C4 1.291(11) . ?
