#------------------------------------------------------------------------------
#$Date: 2019-11-23 04:06:42 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232080 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346947.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_4346947
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         'C30 H22 Co N6, F6 P, 2(C4 H8 O)'
_chemical_formula_sum            'C38 H38 Co F6 N6 O2 P'
_chemical_formula_weight         814.64
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      82
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                WGT-JE-061-03
_audit_creation_date             2012-09-05
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8263(5)
_cell_length_b                   8.8263(5)
_cell_length_c                   27.4049(11)
_cell_measurement_reflns_used    9099
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3992
_cell_measurement_theta_min      2.9742
_cell_volume                     2134.94(19)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_radiation_monochromator  graphite
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            8149
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.95090
_exptl_absorpt_correction_T_min  0.86670
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3057
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0756
_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)+(0.1055P)²+2.5454P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.2018
_reflns_number_gt                2464
_reflns_number_total             3057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02415_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4346947
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
Co Co 1.0000 0.5000 0.7500 0.0317(3) Uani 1 4 d S
N1 N 1.0899(4) 0.7176(4) 0.76815(13) 0.0339(7) Uani 1 1 d .
C2 C 1.1355(4) 0.8248(4) 0.73689(15) 0.0369(9) Uani 1 1 d .
H2 H 1.1250 0.8066 0.7029 0.044 Uiso 1 1 calc R
C3 C 1.1980(4) 0.9622(4) 0.7521(2) 0.0417(8) Uani 1 1 d .
H3 H 1.2321 1.0341 0.7288 0.050 Uiso 1 1 calc R
C4 C 1.2096(6) 0.9922(6) 0.8007(2) 0.0514(12) Uani 1 1 d .
H4 H 1.2499 1.0859 0.8119 0.062 Uiso 1 1 calc R
C5 C 1.1613(7) 0.8832(6) 0.83366(19) 0.0530(12) Uani 1 1 d .
H5 H 1.1684 0.9015 0.8677 0.064 Uiso 1 1 calc R
C6 C 1.1027(5) 0.7476(5) 0.81675(16) 0.0407(9) Uani 1 1 d .
C7 C 1.0497(6) 0.6222(6) 0.84839(17) 0.0510(12) Uani 1 1 d .
C8 C 1.0516(11) 0.6263(9) 0.8987(2) 0.099(3) Uani 1 1 d .
H8 H 1.0872 0.7133 0.9156 0.118 Uiso 1 1 calc R
C9 C 1.0000 0.5000 0.9240(3) 0.119(5) Uani 1 2 d S
H9 H 1.0000 0.5000 0.9587 0.143 Uiso 1 2 calc SR
N10 N 1.0000 0.5000 0.82324(16) 0.0390(9) Uani 1 2 d S
P20 P 1.0000 1.0000 1.0000 0.0689(9) Uani 1 4 d S
F21 F 1.0000 1.0000 0.94177(15) 0.095(2) Uani 1 2 d S
F22 F 0.9402(6) 0.8296(5) 1.00001(17) 0.0961(14) Uani 1 1 d .
O31 O 1.2224(12) 0.8814(11) 0.6254(3) 0.081(3) Uani 0.50 1 d PD
C32 C 1.259(2) 0.8042(16) 0.5844(4) 0.131(10) Uani 0.50 1 d PD
H32A H 1.1747 0.7360 0.5753 0.157 Uiso 0.50 1 calc PR
H32B H 1.3501 0.7415 0.5905 0.157 Uiso 0.50 1 calc PR
C33 C 1.289(2) 0.9112(12) 0.5446(3) 0.088(5) Uani 0.50 1 d PD
H33A H 1.2375 0.8796 0.5141 0.106 Uiso 0.50 1 calc PR
H33B H 1.3990 0.9210 0.5383 0.106 Uiso 0.50 1 calc PR
C34 C 1.225(3) 1.0544(10) 0.5637(4) 0.109(8) Uani 0.50 1 d PD
H34A H 1.1206 1.0722 0.5516 0.130 Uiso 0.50 1 calc PR
H34B H 1.2892 1.1427 0.5556 0.130 Uiso 0.50 1 calc PR
C35 C 1.227(3) 1.0196(19) 0.6178(4) 0.120(9) Uani 0.50 1 d PD
H35A H 1.3204 1.0619 0.6324 0.144 Uiso 0.50 1 calc PR
H35B H 1.1391 1.0687 0.6337 0.144 Uiso 0.50 1 calc PR
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'
Co Co 0.3494 0.9721 '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'
F F 0.0171 0.0103 '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 0.00 0.0300
-1.00 0.00 0.00 0.0300
0.00 0.00 -1.00 0.0600
0.00 0.00 1.00 0.1000
0.00 1.00 1.00 0.1200
0.00 1.00 3.00 0.1000
0.00 -1.00 1.00 0.0750
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
N10 Co N10 180.0 . 7_566
N10 Co N1 76.54(9) . .
N10 Co N1 103.46(9) 7_566 .
N10 Co N1 76.55(9) . 2_765
N10 Co N1 103.45(9) 7_566 2_765
N1 Co N1 153.09(18) . 2_765
N10 Co N1 103.46(9) . 7_566
N10 Co N1 76.54(9) 7_566 7_566
N1 Co N1 93.10(4) . 7_566
N1 Co N1 93.10(4) 2_765 7_566
N10 Co N1 103.46(9) . 8_646
N10 Co N1 76.54(9) 7_566 8_646
N1 Co N1 93.10(4) . 8_646
N1 Co N1 93.10(4) 2_765 8_646
N1 Co N1 153.08(18) 7_566 8_646
C2 N1 C6 117.6(4) . .
C2 N1 Co 126.7(3) . .
C6 N1 Co 115.6(3) . .
N1 C2 C3 122.8(4) . .
C4 C3 C2 119.5(4) . .
C3 C4 C5 118.6(4) . .
C6 C5 C4 119.8(5) . .
N1 C6 C5 121.8(4) . .
N1 C6 C7 113.6(4) . .
C5 C6 C7 124.6(4) . .
N10 C7 C8 122.3(4) . .
N10 C7 C6 113.6(4) . .
C8 C7 C6 124.1(4) . .
C7 C8 C9 118.2(5) . .
C8 C9 C8 120.2(7) . 2_765
C7 N10 C7 118.7(5) 2_765 .
C7 N10 Co 120.6(3) 2_765 .
C7 N10 Co 120.6(3) . .
F22 P20 F22 90.000(3) 3_577 .
F22 P20 F22 180.0(3) 3_577 4_757
F22 P20 F22 90.001(2) . 4_757
F22 P20 F22 89.999(3) 3_577 2_775
F22 P20 F22 180.0(4) . 2_775
F22 P20 F22 90.001(3) 4_757 2_775
F22 P20 F21 90.01(17) 3_577 3_577
F22 P20 F21 89.99(17) . 3_577
F22 P20 F21 90.01(17) 4_757 3_577
F22 P20 F21 89.99(17) 2_775 3_577
F22 P20 F21 89.99(17) 3_577 .
F22 P20 F21 90.01(17) . .
F22 P20 F21 89.99(17) 4_757 .
F22 P20 F21 90.01(17) 2_775 .
F21 P20 F21 180.000(1) 3_577 .
C35 O31 C32 110.4(9) . .
O31 C32 C33 109.7(9) . .
C32 C33 C34 102.5(7) . .
C33 C34 C35 99.7(7) . .
O31 C35 C34 111.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N10 2.007(4) .
Co N10 2.007(4) 7_566
Co N1 2.137(3) .
Co N1 2.137(3) 2_765
Co N1 2.137(3) 7_566
Co N1 2.137(3) 8_646
N1 C2 1.338(5) .
N1 C6 1.363(5) .
C2 C3 1.396(6) .
C3 C4 1.362(8) .
C4 C5 1.386(7) .
C5 C6 1.384(6) .
C6 C7 1.482(6) .
C7 N10 1.353(5) .
C7 C8 1.379(7) .
C8 C9 1.389(7) .
C9 C8 1.389(7) 2_765
N10 C7 1.353(5) 2_765
P20 F22 1.594(5) 3_577
P20 F22 1.594(5) .
P20 F22 1.594(5) 4_757
P20 F22 1.594(5) 2_775
P20 F21 1.596(4) 3_577
P20 F21 1.596(4) .
O31 C35 1.238(17) .
O31 C32 1.353(15) .
C32 C33 1.468(11) .
C33 C34 1.482(12) .
C34 C35 1.514(11) .
