#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:35:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179147 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/08/4310831.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_4310831
loop_
_publ_author_name
'Pauli Kofod'
'Pernille Harris'
_publ_section_title
;
 NMR Spectroscopic and X-ray Crystallographic Study of Methylcobalt(III)
 Compounds with Saturated Amine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2680
_journal_page_last               2688
_journal_paper_doi               10.1021/ic0302682
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C13 H41 Co2 F18 N10 P3'
_chemical_formula_weight         890.33
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.51
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.816(2)
_cell_length_b                   15.903(3)
_cell_length_c                   17.163(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      22.37
_cell_measurement_theta_min      19.2
_cell_volume                     3219.0(12)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'DREADD (Blessing, 1987)'
_computing_molecular_graphics    'OrtepII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12521
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  166.7
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.134
_refine_diff_density_min         -1.515
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.325
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0583
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1788
_reflns_number_gt                7701
_reflns_number_total             9356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0302682_s1_1.cif
_cod_data_source_block           pk39.abs
_cod_database_code               4310831
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.02451(3) 0.11675(2) 0.24602(2) 0.01386(11) Uani 1 1 d . . .
N14 N 0.0071(2) 0.04044(17) 0.33471(17) 0.0264(6) Uani 1 1 d . . .
H14A H -0.0615 0.0130 0.3289 0.040 Uiso 1 1 calc R . .
H14B H 0.0639 0.0008 0.3367 0.040 Uiso 1 1 calc R . .
C1 C 0.1927(2) 0.12835(16) 0.27377(15) 0.0165(5) Uani 0.50 1 d P . .
N1 N 0.1927(2) 0.12835(16) 0.27377(15) 0.0165(5) Uani 0.50 1 d P . .
N12 N 0.0424(2) 0.19426(16) 0.15809(15) 0.0204(5) Uani 1 1 d . . .
H12A H -0.0272 0.2142 0.1396 0.031 Uiso 1 1 calc R . .
H12B H 0.0869 0.2393 0.1741 0.031 Uiso 1 1 calc R . .
N11 N -0.0110(2) 0.20723(16) 0.31845(15) 0.0202(5) Uani 1 1 d . . .
H11A H 0.0528 0.2392 0.3298 0.030 Uiso 1 1 calc R . .
H11B H -0.0660 0.2416 0.2954 0.030 Uiso 1 1 calc R . .
N13 N 0.0559(2) 0.02601(17) 0.17296(17) 0.0247(5) Uani 1 1 d . . .
H13A H 0.1278 0.0053 0.1840 0.037 Uiso 1 1 calc R . .
H13B H 0.0050 -0.0172 0.1778 0.037 Uiso 1 1 calc R . .
C2 C -0.1385(2) 0.10482(19) 0.2153(2) 0.0225(6) Uani 1 1 d . . .
H2A H -0.1819 0.1455 0.2442 0.029 Uiso 1 1 calc R . .
H2B H -0.1633 0.0477 0.2272 0.029 Uiso 1 1 calc R . .
H2C H -0.1511 0.1153 0.1592 0.029 Uiso 1 1 calc R . .
C11 C -0.0514(3) 0.1716(2) 0.3913(2) 0.0304(7) Uani 1 1 d . . .
H11C H -0.1338 0.1604 0.3852 0.039 Uiso 1 1 calc R . .
H11D H -0.0371 0.2116 0.4350 0.039 Uiso 1 1 calc R . .
C12 C 0.0968(3) 0.1468(2) 0.09600(19) 0.0277(7) Uani 1 1 d . . .
H12C H 0.1798 0.1435 0.1080 0.036 Uiso 1 1 calc R . .
H12D H 0.0829 0.1754 0.0451 0.036 Uiso 1 1 calc R . .
C13 C 0.0461(3) 0.0597(2) 0.0928(2) 0.0317(7) Uani 1 1 d . . .
H13C H -0.0344 0.0622 0.0733 0.041 Uiso 1 1 calc R . .
H13D H 0.0876 0.0234 0.0573 0.041 Uiso 1 1 calc R . .
C14 C 0.0129(3) 0.0908(3) 0.4077(2) 0.0343(8) Uani 1 1 d . . .
H14C H 0.0929 0.1031 0.4243 0.045 Uiso 1 1 calc R . .
H14D H -0.0215 0.0591 0.4499 0.045 Uiso 1 1 calc R . .
Co2 Co 0.45739(3) 0.14653(2) 0.31315(2) 0.01373(11) Uani 1 1 d . . .
N24 N 0.4223(2) 0.23548(16) 0.38741(15) 0.0211(5) Uani 1 1 d . . .
H24A H 0.4758 0.2774 0.3862 0.032 Uiso 1 1 calc R . .
H24B H 0.3526 0.2584 0.3733 0.032 Uiso 1 1 calc R . .
N23 N 0.4718(2) 0.22528(16) 0.22595(15) 0.0216(5) Uani 1 1 d . . .
H23A H 0.4115 0.2620 0.2232 0.032 Uiso 1 1 calc R . .
H23B H 0.5375 0.2560 0.2336 0.032 Uiso 1 1 calc R . .
C3 C 0.2897(2) 0.13455(16) 0.28493(15) 0.0166(5) Uani 0.50 1 d P . .
N3 N 0.2897(2) 0.13455(16) 0.28493(15) 0.0166(5) Uani 0.50 1 d P . .
N21 N 0.4938(2) 0.05775(16) 0.23871(15) 0.0204(5) Uani 1 1 d . . .
H21A H 0.5462 0.0213 0.2618 0.031 Uiso 1 1 calc R . .
H21B H 0.4294 0.0277 0.2240 0.031 Uiso 1 1 calc R . .
C4 C 0.6198(2) 0.1580(2) 0.34520(19) 0.0222(6) Uani 1 1 d . . .
H4A H 0.6637 0.1180 0.3158 0.029 Uiso 1 1 calc R . .
H4B H 0.6315 0.1464 0.4012 0.029 Uiso 1 1 calc R . .
H4C H 0.6448 0.2154 0.3345 0.029 Uiso 1 1 calc R . .
N22 N 0.4443(2) 0.06875(16) 0.40124(15) 0.0228(5) Uani 1 1 d . . .
H22A H 0.4074 0.0205 0.3845 0.034 Uiso 1 1 calc R . .
H22B H 0.5153 0.0543 0.4220 0.034 Uiso 1 1 calc R . .
C21 C 0.5402(3) 0.0971(2) 0.16930(19) 0.0267(6) Uani 1 1 d . . .
H21C H 0.5324 0.0584 0.1241 0.035 Uiso 1 1 calc R . .
H21D H 0.6216 0.1102 0.1798 0.035 Uiso 1 1 calc R . .
C22 C 0.3794(3) 0.1115(2) 0.46116(19) 0.0279(7) Uani 1 1 d . . .
H22C H 0.3916 0.0826 0.5121 0.036 Uiso 1 1 calc R . .
H22D H 0.2974 0.1106 0.4456 0.036 Uiso 1 1 calc R . .
C23 C 0.4738(3) 0.1766(2) 0.15221(19) 0.0270(6) Uani 1 1 d . . .
H23C H 0.5101 0.2101 0.1120 0.035 Uiso 1 1 calc R . .
H23D H 0.3955 0.1628 0.1325 0.035 Uiso 1 1 calc R . .
C24 C 0.4214(3) 0.2007(2) 0.46745(19) 0.0284(7) Uani 1 1 d . . .
H24C H 0.3708 0.2345 0.4990 0.037 Uiso 1 1 calc R . .
H24D H 0.4987 0.2021 0.4931 0.037 Uiso 1 1 calc R . .
P1 P 0.32043(7) 0.89738(5) 0.09010(5) 0.02055(17) Uani 1 1 d . . .
F1 F 0.32595(17) 0.79733(12) 0.07750(12) 0.0292(4) Uani 1 1 d . . .
F2 F 0.31307(17) 0.99761(12) 0.10531(14) 0.0332(5) Uani 1 1 d . . .
F3 F 0.2309(2) 0.88337(14) 0.15530(14) 0.0367(5) Uani 1 1 d . . .
F4 F 0.42209(18) 0.89100(12) 0.15641(13) 0.0329(5) Uani 1 1 d . . .
F5 F 0.2185(2) 0.90353(15) 0.02544(14) 0.0403(6) Uani 1 1 d . . .
F6 F 0.4100(2) 0.91229(17) 0.02670(15) 0.0440(6) Uani 1 1 d . . .
P2 P 0.26121(7) 0.37111(5) 0.09043(5) 0.02330(17) Uani 1 1 d . . .
F7 F 0.39613(19) 0.36664(14) 0.10156(16) 0.0385(5) Uani 1 1 d . . .
F8 F 0.12588(19) 0.37526(14) 0.08076(15) 0.0396(5) Uani 1 1 d . . .
F9 F 0.25221(17) 0.30763(13) 0.16305(11) 0.0290(4) Uani 1 1 d . . .
F10 F 0.26079(18) 0.45020(13) 0.14885(14) 0.0353(5) Uani 1 1 d . . .
F11 F 0.2603(2) 0.29215(14) 0.03291(13) 0.0408(5) Uani 1 1 d . . .
F12 F 0.2697(2) 0.43423(16) 0.01910(15) 0.0498(7) Uani 1 1 d . . .
P3 P 0.26327(8) 0.12874(5) 0.68111(5) 0.02581(19) Uani 1 1 d . . .
F13 F 0.1367(2) 0.11675(17) 0.70991(16) 0.0466(6) Uani 1 1 d . . .
F14 F 0.3017(2) 0.05668(17) 0.7426(2) 0.0588(8) Uani 1 1 d . . .
F16 F 0.2884(3) 0.19433(18) 0.75114(17) 0.0565(8) Uani 1 1 d . . .
F15 F 0.2367(3) 0.0607(2) 0.61626(19) 0.0824(12) Uani 1 1 d . . .
F17 F 0.3874(3) 0.1415(3) 0.6561(2) 0.0919(14) Uani 1 1 d . . .
F18 F 0.2232(4) 0.2009(3) 0.6258(3) 0.1115(17) Uani 1 1 d . . .
N31 N 0.8949(3) 0.88029(19) 0.10755(19) 0.0324(6) Uani 1 1 d . . .
C31 C 0.8006(3) 0.88602(19) 0.09066(19) 0.0250(6) Uani 1 1 d . . .
C32 C 0.6797(3) 0.8927(3) 0.0670(2) 0.0345(8) 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'
Co Co 0.3494 0.9721 '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'
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'
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
N13 Co1 N11 178.57(10) . . ?
N13 Co1 N14 94.23(13) . . ?
N11 Co1 N14 85.73(12) . . ?
N13 Co1 N12 86.40(12) . . ?
N11 Co1 N12 93.65(11) . . ?
N14 Co1 N12 179.32(12) . . ?
N13 Co1 C2 88.75(12) . . ?
N11 Co1 C2 89.82(12) . . ?
N14 Co1 C2 90.04(13) . . ?
N12 Co1 C2 90.26(12) . . ?
N13 Co1 C1 89.77(10) . . ?
N11 Co1 C1 91.66(10) . . ?
N14 Co1 C1 91.26(11) . . ?
N12 Co1 C1 88.46(10) . . ?
C2 Co1 C1 178.10(12) . . ?
C14 N14 Co1 108.6(2) . . ?
C3 C1 Co1 175.9(2) . . ?
C12 N12 Co1 107.7(2) . . ?
C11 N11 Co1 110.3(2) . . ?
C13 N13 Co1 108.8(2) . . ?
N11 C11 C14 107.4(3) . . ?
N12 C12 C13 107.7(3) . . ?
N13 C13 C12 106.9(3) . . ?
N14 C14 C11 107.8(3) . . ?
N24 Co2 N23 93.82(11) . . ?
N24 Co2 N22 85.67(11) . . ?
N23 Co2 N22 179.24(11) . . ?
N24 Co2 N21 179.53(11) . . ?
N23 Co2 N21 86.01(11) . . ?
N22 Co2 N21 94.50(11) . . ?
N24 Co2 C4 89.57(12) . . ?
N23 Co2 C4 91.46(12) . . ?
N22 Co2 C4 87.97(12) . . ?
N21 Co2 C4 90.00(12) . . ?
N24 Co2 C3 88.90(10) . . ?
N23 Co2 C3 90.39(10) . . ?
N22 Co2 C3 90.17(11) . . ?
N21 Co2 C3 91.54(10) . . ?
C4 Co2 C3 177.68(12) . . ?
C24 N24 Co2 110.29(19) . . ?
C23 N23 Co2 108.88(19) . . ?
C1 C3 Co2 175.6(2) . . ?
C21 N21 Co2 109.0(2) . . ?
C22 N22 Co2 108.21(19) . . ?
N21 C21 C23 107.2(3) . . ?
N22 C22 C24 107.5(3) . . ?
N23 C23 C21 107.8(3) . . ?
N24 C24 C22 107.8(2) . . ?
F6 P1 F5 91.20(15) . . ?
F6 P1 F3 179.02(15) . . ?
F5 P1 F3 89.51(15) . . ?
F6 P1 F4 89.65(14) . . ?
F5 P1 F4 179.15(15) . . ?
F3 P1 F4 89.64(14) . . ?
F6 P1 F1 91.23(13) . . ?
F5 P1 F1 90.13(11) . . ?
F3 P1 F1 89.45(12) . . ?
F4 P1 F1 89.89(11) . . ?
F6 P1 F2 90.46(14) . . ?
F5 P1 F2 90.35(12) . . ?
F3 P1 F2 88.85(12) . . ?
F4 P1 F2 89.61(11) . . ?
F1 P1 F2 178.23(13) . . ?
F12 P2 F7 90.62(14) . . ?
F12 P2 F11 91.08(14) . . ?
F7 P2 F11 90.43(14) . . ?
F12 P2 F8 90.22(14) . . ?
F7 P2 F8 179.05(15) . . ?
F11 P2 F8 89.98(13) . . ?
F12 P2 F10 89.38(14) . . ?
F7 P2 F10 90.08(12) . . ?
F11 P2 F10 179.31(15) . . ?
F8 P2 F10 89.50(12) . . ?
F12 P2 F9 179.61(15) . . ?
F7 P2 F9 89.55(12) . . ?
F11 P2 F9 89.27(12) . . ?
F8 P2 F9 89.60(13) . . ?
F10 P2 F9 90.28(12) . . ?
F18 P3 F17 89.6(3) . . ?
F18 P3 F15 92.0(2) . . ?
F17 P3 F15 92.56(19) . . ?
F18 P3 F14 176.7(2) . . ?
F17 P3 F14 92.3(2) . . ?
F15 P3 F14 90.6(2) . . ?
F18 P3 F16 90.7(2) . . ?
F17 P3 F16 89.32(17) . . ?
F15 P3 F16 176.66(18) . . ?
F14 P3 F16 86.55(18) . . ?
F18 P3 F13 91.2(2) . . ?
F17 P3 F13 178.02(18) . . ?
F15 P3 F13 89.25(16) . . ?
F14 P3 F13 86.83(15) . . ?
F16 P3 F13 88.84(15) . . ?
N31 C31 C32 178.6(4) . . ?
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 N13 1.962(3) . ?
Co1 N11 1.964(2) . ?
Co1 N14 1.967(3) . ?
Co1 N12 1.970(3) . ?
Co1 C2 1.974(3) . ?
Co1 C1 2.023(3) . ?
N14 C14 1.484(5) . ?
C1 C3 1.155(4) . ?
N12 C12 1.484(4) . ?
N11 C11 1.478(4) . ?
N13 C13 1.475(5) . ?
C11 C14 1.511(5) . ?
C12 C13 1.509(5) . ?
Co2 N24 1.965(2) . ?
Co2 N23 1.967(3) . ?
Co2 N22 1.967(3) . ?
Co2 N21 1.969(2) . ?
Co2 C4 1.972(3) . ?
Co2 C3 2.020(3) . ?
N24 C24 1.481(4) . ?
N23 C23 1.485(4) . ?
N21 C21 1.480(4) . ?
N22 C22 1.485(4) . ?
C21 C23 1.509(5) . ?
C22 C24 1.504(5) . ?
P1 F6 1.582(2) . ?
P1 F5 1.590(2) . ?
P1 F3 1.602(2) . ?
P1 F4 1.607(2) . ?
P1 F1 1.608(2) . ?
P1 F2 1.618(2) . ?
P2 F12 1.591(2) . ?
P2 F7 1.596(2) . ?
P2 F11 1.597(2) . ?
P2 F8 1.599(2) . ?
P2 F10 1.609(2) . ?
P2 F9 1.613(2) . ?
P3 F18 1.545(3) . ?
P3 F17 1.566(3) . ?
P3 F15 1.570(3) . ?
P3 F14 1.605(3) . ?
P3 F16 1.605(3) . ?
P3 F13 1.615(3) . ?
N31 C31 1.137(5) . ?
C31 C32 1.465(5) . ?
