#------------------------------------------------------------------------------
#$Date: 2019-11-23 04:06:42 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232080 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346952.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_4346952
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_compound_source        'acetonitrile, diethylether'
_chemical_formula_moiety         'C36 H24 Co N6, B F4, 3.5(C2 H3 N)'
_chemical_formula_sum            'C43 H34.5 B Co F4 N9.5'
_chemical_formula_weight         830.04
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_block_code                WGT-JE-096-01
_audit_creation_date             2014-02-26
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.2287(11)
_cell_length_b                   14.2287(11)
_cell_length_c                   34.0196(13)
_cell_measurement_reflns_used    28834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0947
_cell_measurement_theta_min      2.8633
_cell_volume                     5964.7(7)
_computing_cell_refinement       'REVALCCD V. 1.6, 2008'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'REVALCCD V. 1.6, 2008'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_radiation_monochromator  'Incoatec Helios focusing multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            27336
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.091
_diffrn_reflns_theta_min         2.863
_diffrn_source                   '0.2 x 2mm^2^ focus rotating anode'
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.94317
_exptl_absorpt_correction_T_min  0.92935
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             2562
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0364
_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)+(0.0452P)²+8.8774P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4611
_reflns_number_total             5031
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02415_si_002.cif
_cod_data_source_block           9
_cod_original_cell_volume        5964.7(9)
_cod_original_formula_sum        'C43 H34.50 B Co F4 N9.50'
_cod_database_code               4346952
_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.
;
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.934
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Co Co 0.3333 0.6667 0.37482(2) 0.01324(6) Uani 1 3 d S T P
N1 N 0.41210(7) 0.60021(7) 0.40769(2) 0.01506(14) Uani 1 1 d . . .
C2 C 0.46732(8) 0.63618(9) 0.44146(3) 0.01809(17) Uani 1 1 d . . .
H2 H 0.4683 0.6961 0.4542 0.022 Uiso 1 1 calc R U .
C3 C 0.52366(9) 0.58961(9) 0.45886(3) 0.02155(19) Uani 1 1 d . . .
H3 H 0.5619 0.6181 0.4828 0.026 Uiso 1 1 calc R U .
C4 C 0.52349(9) 0.50221(9) 0.44113(3) 0.0222(2) Uani 1 1 d . . .
H4 H 0.5617 0.4702 0.4526 0.027 Uiso 1 1 calc R U .
C5 C 0.46548(8) 0.46133(8) 0.40563(3) 0.01891(18) Uani 1 1 d . . .
C6 C 0.46048(10) 0.37126(9) 0.38462(4) 0.0243(2) Uani 1 1 d . . .
H6 H 0.4974 0.3363 0.3947 0.029 Uiso 1 1 calc R U .
C7 C 0.40369(10) 0.33539(9) 0.35047(4) 0.0246(2) Uani 1 1 d . . .
H7 H 0.4012 0.2754 0.3372 0.030 Uiso 1 1 calc R U .
C8 C 0.34739(9) 0.38667(8) 0.33413(3) 0.01953(18) Uani 1 1 d . . .
C9 C 0.28679(10) 0.35244(9) 0.29897(3) 0.0233(2) Uani 1 1 d . . .
H9 H 0.2816 0.2927 0.2846 0.028 Uiso 1 1 calc R U .
C10 C 0.23516(9) 0.40657(9) 0.28559(3) 0.0228(2) Uani 1 1 d . . .
H10 H 0.1936 0.3842 0.2621 0.027 Uiso 1 1 calc R U .
C11 C 0.24489(9) 0.49501(9) 0.30714(3) 0.01964(18) Uani 1 1 d . . .
H11 H 0.2093 0.5318 0.2975 0.024 Uiso 1 1 calc R U .
N12 N 0.30179(7) 0.53040(7) 0.34064(2) 0.01584(15) Uani 1 1 d . . .
C13 C 0.35158(8) 0.47572(8) 0.35404(3) 0.01566(16) Uani 1 1 d . . .
C14 C 0.41103(8) 0.51326(8) 0.39020(3) 0.01532(16) Uani 1 1 d . . .
B20 B 0.3333 0.6667 0.54219(7) 0.0221(4) Uani 1 3 d S T P
F21 F 0.3333 0.6667 0.58287(5) 0.0429(4) Uani 1 3 d S T P
F22 F 0.43968(7) 0.71574(8) 0.52887(3) 0.0410(2) Uani 1 1 d . . .
N30 N 0.7877(3) 0.6853(3) 0.52508(6) 0.0912(9) Uani 1 1 d . . .
C31 C 0.80775(18) 0.68788(17) 0.49285(6) 0.0532(5) Uani 1 1 d . . .
C32 C 0.83341(17) 0.68999(17) 0.45142(6) 0.0518(4) Uani 1 1 d . . .
H32A H 0.7846 0.6190 0.4397 0.078 Uiso 1 1 calc R U .
H32B H 0.9087 0.7064 0.4486 0.078 Uiso 1 1 calc R U .
H32C H 0.8243 0.7459 0.4380 0.078 Uiso 1 1 calc R U .
N40 N 1.0000 1.0000 0.4465(3) 0.137(5) Uani 0.5 3 d DS TU P
C41 C 1.0000 1.0000 0.4795(3) 0.131(6) Uani 0.5 3 d DS TU P
C42 C 1.0000 1.0000 0.5215(3) 0.080(3) Uani 0.5 3 d DS TU P
H42A H 1.0750 1.0380 0.5311 0.120 Uiso 0.1667 1 calc R U P
H42B H 0.9630 0.9250 0.5311 0.120 Uiso 0.1667 1 calc R U P
H42C H 0.9620 1.0370 0.5311 0.120 Uiso 0.1667 1 calc R U P
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'
B B 0.0013 0.0007 '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'
Co Co 0.3494 0.9721 '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 -1.00 3.00 0.0700
-1.00 1.00 -3.00 0.0700
0.00 -1.00 -2.00 0.1000
0.00 1.00 2.00 0.0900
1.00 -2.00 1.00 0.0900
-1.00 2.00 -1.00 0.0900
-1.00 0.00 2.00 0.1000
2.00 -1.00 -4.00 0.0600
-1.00 1.00 5.00 0.0900
1.00 1.00 -1.00 0.0800
-1.00 -1.00 -1.00 0.1000
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 Co N12 92.48(3) . 3_565
N12 Co N12 92.48(3) . 2_665
N12 Co N12 92.48(3) 3_565 2_665
N12 Co N1 78.28(3) . .
N12 Co N1 167.78(3) 3_565 .
N12 Co N1 95.86(3) 2_665 .
N12 Co N1 167.78(3) . 2_665
N12 Co N1 95.86(3) 3_565 2_665
N12 Co N1 78.28(3) 2_665 2_665
N1 Co N1 94.56(3) . 2_665
N12 Co N1 95.86(3) . 3_565
N12 Co N1 78.28(3) 3_565 3_565
N12 Co N1 167.78(3) 2_665 3_565
N1 Co N1 94.56(3) . 3_565
N1 Co N1 94.56(3) 2_665 3_565
C2 N1 C14 117.26(9) . .
C2 N1 Co 128.59(7) . .
C14 N1 Co 114.00(6) . .
N1 C2 C3 123.11(10) . .
C4 C3 C2 119.82(10) . .
C3 C4 C5 118.80(10) . .
C14 C5 C4 117.54(9) . .
C14 C5 C6 119.08(10) . .
C4 C5 C6 123.37(10) . .
C7 C6 C5 120.95(10) . .
C6 C7 C8 121.12(10) . .
C9 C8 C13 117.45(10) . .
C9 C8 C7 123.49(10) . .
C13 C8 C7 119.07(10) . .
C10 C9 C8 119.38(10) . .
C9 C10 C11 119.15(10) . .
N12 C11 C10 123.45(10) . .
C11 N12 C13 117.20(9) . .
C11 N12 Co 128.68(7) . .
C13 N12 Co 114.03(6) . .
N12 C13 C8 123.37(9) . .
N12 C13 C14 116.79(8) . .
C8 C13 C14 119.84(9) . .
N1 C14 C5 123.47(9) . .
N1 C14 C13 116.60(8) . .
C5 C14 C13 119.93(9) . .
F21 B20 F22 109.05(10) . 2_665
F21 B20 F22 109.05(10) . 3_565
F22 B20 F22 109.88(10) 2_665 3_565
F21 B20 F22 109.06(10) . .
F22 B20 F22 109.88(10) 2_665 .
F22 B20 F22 109.88(10) 3_565 .
N30 C31 C32 179.3(2) . .
N40 C41 C42 180.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N12 2.1079(9) .
Co N12 2.1080(9) 3_565
Co N12 2.1079(9) 2_665
Co N1 2.1119(9) .
Co N1 2.1119(9) 2_665
Co N1 2.1119(9) 3_565
N1 C2 1.3405(13) .
N1 C14 1.3661(12) .
C2 C3 1.4013(14) .
C3 C4 1.3810(16) .
C4 C5 1.4135(16) .
C5 C14 1.4122(14) .
C5 C6 1.4376(16) .
C6 C7 1.3604(18) .
C7 C8 1.4381(16) .
C8 C9 1.4112(16) .
C8 C13 1.4113(14) .
C9 C10 1.3806(17) .
C10 C11 1.4022(15) .
C11 N12 1.3417(13) .
N12 C13 1.3661(13) .
C13 C14 1.4362(14) .
B20 F21 1.384(3) .
B20 F22 1.3878(11) 2_665
B20 F22 1.3878(11) 3_565
B20 F22 1.3879(11) .
N30 C31 1.129(3) .
C31 C32 1.453(3) .
N40 C41 1.124(5) .
C41 C42 1.429(5) .
