#------------------------------------------------------------------------------
#$Date: 2019-11-23 04:06:42 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232080 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346944.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_4346944
loop_
_publ_author_name
'England, Jason'
'Bill, Eckhard'
'Weyhermüller, Thomas'
'Neese, Frank'
'Atanasov, Mihail'
'Wieghardt, Karl'
_publ_section_title
;
 Molecular and Electronic Structures of Homoleptic Six-Coordinate
 Cobalt(I) Complexes of 2,2':6',2″-Terpyridine, 2,2'-Bipyridine,
 and 1,10-Phenanthroline. An Experimental and Computational Study.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12002
_journal_page_last               12018
_journal_paper_doi               10.1021/acs.inorgchem.5b02415
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C44 H34 Co N6, 2(C3 H6 O), 3(F6 P)'
_chemical_formula_sum            'C50 H46 Co F18 N6 O2 P3'
_chemical_formula_weight         1256.77
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_block_code                WGT-CA-054-02
_audit_creation_date             2011-10-06
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.593(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.487(2)
_cell_length_b                   16.240(2)
_cell_length_c                   20.746(3)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2851
_cell_measurement_theta_min      2.2181
_cell_volume                     5111.4(12)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            68350
_diffrn_reflns_theta_full        30.63
_diffrn_reflns_theta_max         30.63
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.98399
_exptl_absorpt_correction_T_min  0.94632
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.349
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0546
_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)+(0.0714P)²+15.7407P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                6144
_reflns_number_total             7841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02415_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     '-c 2yc'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4346944
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 0.21023(3) 0.2500 0.01641(10) Uani 1 2 d S
N1 N 0.47624(12) 0.29409(11) 0.31144(9) 0.0189(3) Uani 1 1 d .
C2 C 0.39967(15) 0.33256(14) 0.31094(11) 0.0216(4) Uani 1 1 d .
H2 H 0.3497 0.3185 0.2781 0.026 Uiso 1 1 calc R
C3 C 0.39115(16) 0.39242(15) 0.35715(12) 0.0246(5) Uani 1 1 d .
H3 H 0.3360 0.4185 0.3562 0.030 Uiso 1 1 calc R
C4 C 0.46390(17) 0.41353(16) 0.40450(13) 0.0271(5) Uani 1 1 d .
H4 H 0.4593 0.4545 0.4363 0.032 Uiso 1 1 calc R
C5 C 0.54375(16) 0.37437(15) 0.40525(12) 0.0250(5) Uani 1 1 d .
H5 H 0.5945 0.3883 0.4374 0.030 Uiso 1 1 calc R
C6 C 0.54831(15) 0.31469(14) 0.35849(11) 0.0203(4) Uani 1 1 d .
C7 C 0.62820(14) 0.26873(13) 0.35291(11) 0.0194(4) Uani 1 1 d .
C8 C 0.71278(15) 0.27832(14) 0.38928(11) 0.0213(4) Uani 1 1 d .
H8 H 0.7241 0.3168 0.4245 0.026 Uiso 1 1 calc R
C9 C 0.78198(14) 0.23101(14) 0.37402(11) 0.0205(4) Uani 1 1 d .
C10 C 0.76195(15) 0.17367(14) 0.32214(11) 0.0212(4) Uani 1 1 d .
H10 H 0.8072 0.1409 0.3104 0.025 Uiso 1 1 calc R
C11 C 0.67579(14) 0.16568(14) 0.28845(11) 0.0195(4) Uani 1 1 d .
N12 N 0.61156(12) 0.21296(11) 0.30397(9) 0.0185(3) Uani 1 1 d .
C13 C 0.64119(15) 0.11110(14) 0.23245(11) 0.0209(4) Uani 1 1 d .
C14 C 0.68921(17) 0.05029(16) 0.20896(13) 0.0289(5) Uani 1 1 d .
H14 H 0.7495 0.0414 0.2284 0.035 Uiso 1 1 calc R
C15 C 0.64727(18) 0.00218(18) 0.15612(14) 0.0338(6) Uani 1 1 d .
H15 H 0.6786 -0.0404 0.1393 0.041 Uiso 1 1 calc R
C16 C 0.55964(17) 0.01696(16) 0.12834(13) 0.0285(5) Uani 1 1 d .
H16 H 0.5305 -0.0150 0.0921 0.034 Uiso 1 1 calc R
C17 C 0.51465(15) 0.07903(15) 0.15401(11) 0.0229(4) Uani 1 1 d .
H17 H 0.4545 0.0891 0.1349 0.027 Uiso 1 1 calc R
N18 N 0.55441(12) 0.12512(11) 0.20526(9) 0.0189(3) Uani 1 1 d .
C19 C 0.87309(15) 0.24140(15) 0.41151(11) 0.0220(4) Uani 1 1 d .
C20 C 0.89780(16) 0.31225(16) 0.44895(12) 0.0248(5) Uani 1 1 d .
H20 H 0.8557 0.3547 0.4494 0.030 Uiso 1 1 calc R
C21 C 0.98226(16) 0.32180(16) 0.48531(12) 0.0268(5) Uani 1 1 d .
H21 H 0.9975 0.3708 0.5101 0.032 Uiso 1 1 calc R
C22 C 1.04541(16) 0.26056(16) 0.48615(12) 0.0263(5) Uani 1 1 d .
C23 C 1.02184(17) 0.19019(17) 0.44841(13) 0.0288(5) Uani 1 1 d .
H23 H 1.0643 0.1481 0.4481 0.035 Uiso 1 1 calc R
C24 C 0.93714(16) 0.18045(15) 0.41120(12) 0.0257(5) Uani 1 1 d .
H24 H 0.9226 0.1322 0.3854 0.031 Uiso 1 1 calc R
C25 C 1.13619(17) 0.27101(18) 0.52753(14) 0.0333(6) Uani 1 1 d .
H25A H 1.1672 0.2181 0.5312 0.050 Uiso 1 1 calc R
H25B H 1.1316 0.2903 0.5715 0.050 Uiso 1 1 calc R
H25C H 1.1690 0.3115 0.5069 0.050 Uiso 1 1 calc R
P30 P 0.27008(4) 0.01153(4) 0.03860(3) 0.02773(15) Uani 1 1 d .
F31 F 0.17442(13) 0.03811(14) 0.04722(11) 0.0546(6) Uani 1 1 d .
F32 F 0.29660(16) -0.00101(15) 0.11706(10) 0.0574(6) Uani 1 1 d .
F33 F 0.30302(18) 0.10521(13) 0.05019(12) 0.0662(7) Uani 1 1 d .
F34 F 0.24458(13) 0.02774(14) -0.03825(9) 0.0484(5) Uani 1 1 d .
F35 F 0.24105(15) -0.08130(11) 0.03090(11) 0.0538(5) Uani 1 1 d .
F36 F 0.36752(11) -0.01258(14) 0.03069(10) 0.0494(5) Uani 1 1 d .
P40 P 0.5000 0.55580(6) 0.2500 0.02792(19) Uani 1 2 d S
F41 F 0.40554(11) 0.55575(12) 0.27098(10) 0.0445(4) Uani 1 1 d .
F42 F 0.54765(12) 0.55620(11) 0.32584(9) 0.0414(4) Uani 1 1 d .
F43 F 0.5000 0.45774(13) 0.2500 0.0341(5) Uani 1 2 d S
F44 F 0.5000 0.65458(15) 0.2500 0.0489(7) Uani 1 2 d S
O50 O 0.18752(16) 0.33996(16) 0.26229(12) 0.0498(6) Uani 1 1 d .
C51 C 0.15212(19) 0.3123(2) 0.30528(15) 0.0395(7) Uani 1 1 d .
C52 C 0.0749(2) 0.3532(3) 0.3250(2) 0.0532(9) Uani 1 1 d .
H52A H 0.0602 0.4037 0.2993 0.080 Uiso 1 1 calc R
H52B H 0.0896 0.3668 0.3720 0.080 Uiso 1 1 calc R
H52C H 0.0242 0.3158 0.3167 0.080 Uiso 1 1 calc R
C53 C 0.1825(2) 0.2354(2) 0.34097(17) 0.0445(7) Uani 1 1 d .
H53A H 0.2393 0.2190 0.3311 0.067 Uiso 1 1 calc R
H53B H 0.1391 0.1917 0.3271 0.067 Uiso 1 1 calc R
H53C H 0.1892 0.2446 0.3884 0.067 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 -1.00 0.0400
-1.00 0.00 1.00 0.0400
1.00 0.00 1.00 0.0250
-1.00 0.00 -1.00 0.0250
-2.00 2.00 1.00 0.0200
2.00 -2.00 -1.00 0.0200
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
N12 Co1 N12 177.27(12) 2_655 .
N12 Co1 N18 82.26(8) 2_655 2_655
N12 Co1 N18 99.70(8) . 2_655
N12 Co1 N18 99.69(8) 2_655 .
N12 Co1 N18 82.27(8) . .
N18 Co1 N18 89.64(11) 2_655 .
N12 Co1 N1 82.21(8) 2_655 2_655
N12 Co1 N1 95.87(8) . 2_655
N18 Co1 N1 164.41(8) 2_655 2_655
N18 Co1 N1 91.58(8) . 2_655
N12 Co1 N1 95.87(8) 2_655 .
N12 Co1 N1 82.21(8) . .
N18 Co1 N1 91.58(8) 2_655 .
N18 Co1 N1 164.41(8) . .
N1 Co1 N1 91.41(11) 2_655 .
C2 N1 C6 119.07(19) . .
C2 N1 Co1 127.16(16) . .
C6 N1 Co1 113.76(14) . .
N1 C2 C3 121.9(2) . .
C4 C3 C2 119.2(2) . .
C3 C4 C5 119.5(2) . .
C6 C5 C4 119.0(2) . .
N1 C6 C5 121.5(2) . .
N1 C6 C7 113.50(19) . .
C5 C6 C7 125.0(2) . .
N12 C7 C8 120.3(2) . .
N12 C7 C6 111.38(19) . .
C8 C7 C6 128.3(2) . .
C7 C8 C9 119.8(2) . .
C8 C9 C10 118.2(2) . .
C8 C9 C19 120.7(2) . .
C10 C9 C19 121.2(2) . .
C11 C10 C9 119.3(2) . .
N12 C11 C10 120.7(2) . .
N12 C11 C13 111.25(19) . .
C10 C11 C13 128.0(2) . .
C11 N12 C7 121.70(19) . .
C11 N12 Co1 118.94(15) . .
C7 N12 Co1 118.93(15) . .
N18 C13 C14 121.8(2) . .
N18 C13 C11 113.35(19) . .
C14 C13 C11 124.8(2) . .
C13 C14 C15 118.6(2) . .
C16 C15 C14 119.5(2) . .
C15 C16 C17 119.4(2) . .
N18 C17 C16 121.4(2) . .
C17 N18 C13 119.30(19) . .
C17 N18 Co1 126.77(16) . .
C13 N18 Co1 113.87(15) . .
C20 C19 C24 117.9(2) . .
C20 C19 C9 120.8(2) . .
C24 C19 C9 121.2(2) . .
C21 C20 C19 121.3(2) . .
C20 C21 C22 120.8(2) . .
C23 C22 C21 118.4(2) . .
C23 C22 C25 121.6(2) . .
C21 C22 C25 120.0(2) . .
C24 C23 C22 121.1(2) . .
C23 C24 C19 120.4(2) . .
F35 P30 F34 92.79(12) . .
F35 P30 F31 91.03(12) . .
F34 P30 F31 91.07(11) . .
F35 P30 F36 90.64(12) . .
F34 P30 F36 89.25(11) . .
F31 P30 F36 178.28(13) . .
F35 P30 F33 176.95(15) . .
F34 P30 F33 90.04(13) . .
F31 P30 F33 90.06(13) . .
F36 P30 F33 88.25(13) . .
F35 P30 F32 89.49(12) . .
F34 P30 F32 177.70(13) . .
F31 P30 F32 88.55(12) . .
F36 P30 F32 91.06(12) . .
F33 P30 F32 87.69(13) . .
F43 P40 F42 90.23(7) . .
F43 P40 F42 90.23(7) . 2_655
F42 P40 F42 179.53(14) . 2_655
F43 P40 F44 180.000(1) . .
F42 P40 F44 89.77(7) . .
F42 P40 F44 89.77(7) 2_655 .
F43 P40 F41 89.97(8) . .
F42 P40 F41 89.92(10) . .
F42 P40 F41 90.08(10) 2_655 .
F44 P40 F41 90.03(8) . .
F43 P40 F41 89.97(8) . 2_655
F42 P40 F41 90.08(10) . 2_655
F42 P40 F41 89.92(10) 2_655 2_655
F44 P40 F41 90.03(8) . 2_655
F41 P40 F41 179.95(17) . 2_655
O50 C51 C53 122.1(3) . .
O50 C51 C52 122.5(3) . .
C53 C51 C52 115.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N12 1.8609(19) 2_655
Co1 N12 1.8609(19) .
Co1 N18 1.9483(19) 2_655
Co1 N18 1.9484(19) .
Co1 N1 1.9502(19) 2_655
Co1 N1 1.9503(19) .
N1 C2 1.339(3) .
N1 C6 1.368(3) .
C2 C3 1.390(3) .
C3 C4 1.381(4) .
C4 C5 1.388(3) .
C5 C6 1.383(3) .
C6 C7 1.469(3) .
C7 N12 1.346(3) .
C7 C8 1.383(3) .
C8 C9 1.405(3) .
C9 C10 1.410(3) .
C9 C19 1.478(3) .
C10 C11 1.382(3) .
C11 N12 1.346(3) .
C11 C13 1.474(3) .
C13 N18 1.368(3) .
C13 C14 1.383(3) .
C14 C15 1.396(4) .
C15 C16 1.385(4) .
C16 C17 1.391(3) .
C17 N18 1.344(3) .
C19 C20 1.398(3) .
C19 C24 1.402(3) .
C20 C21 1.381(3) .
C21 C22 1.393(4) .
C22 C23 1.392(4) .
C22 C25 1.503(4) .
C23 C24 1.391(3) .
P30 F35 1.5722(19) .
P30 F34 1.5855(19) .
P30 F31 1.5873(19) .
P30 F36 1.5992(19) .
P30 F33 1.607(2) .
P30 F32 1.610(2) .
P40 F43 1.593(2) .
P40 F42 1.5979(18) .
P40 F42 1.5980(18) 2_655
P40 F44 1.604(3) .
P40 F41 1.6079(17) .
P40 F41 1.6080(17) 2_655
O50 C51 1.223(4) .
C51 C53 1.479(5) .
C51 C52 1.496(4) .
