#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:19:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178559 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/67/4066751.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_4066751
loop_
_publ_author_name
'Aguirre-Etcheverry, Paulina'
'Ashley, Andrew E.'
'Balázs, Gábor'
'Green, Jennifer C.'
'Cowley, Andrew R.'
'Thompson, Amber L.'
'O’Hare, Dermot'
_publ_section_title
;
 Synthesis, Structure, and Ligand Exchange Reactions of
 Tetramethyleneethane Complexes of Cobalt
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5847
_journal_paper_doi               10.1021/om100611p
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C34 H62 Co2 O4 P2'
_chemical_formula_sum            'C34 H62 Co2 O4 P2'
_chemical_formula_weight         714.64
_chemical_melting_point          ?
_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
_cell_angle_alpha                93.519(1)
_cell_angle_beta                 102.906(1)
_cell_angle_gamma                101.657(1)
_cell_formula_units_Z            1
_cell_length_a                   9.7293(2)
_cell_length_b                   9.7312(2)
_cell_length_c                   10.5514(3)
_cell_measurement_reflns_used    3852
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      2.910
_cell_volume                     947.71(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0887
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7260
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_correction_T_min  0.9429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_orange
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4148
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0443
_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)+(0.0337P)²+0.0641P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                2845
_reflns_number_total             4148
_reflns_threshold_expression     >2sigma(I)
_oxford_structure_analysis_title 5406
_cod_data_source_file            om100611p_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066751
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
Co1 Co 0.50346(4) 0.19512(4) 0.36207(4) 0.02422(13) Uani 1 1 d .
O1 O 0.5857(3) 0.5021(2) 0.3670(2) 0.0465(6) Uani 1 1 d .
O2 O 0.6733(2) 0.0735(2) 0.2096(2) 0.0419(6) Uani 1 1 d .
C1 C 0.5468(3) 0.3818(3) 0.3685(3) 0.0305(7) Uani 1 1 d .
C2 C 0.6032(3) 0.1202(3) 0.2693(3) 0.0287(7) Uani 1 1 d .
C3 C 0.6392(4) 0.1797(3) 0.5375(3) 0.0330(7) Uani 1 1 d D
H3A H 0.652(3) 0.267(2) 0.597(3) 0.040 Uiso 1 1 d D
H3B H 0.730(2) 0.152(3) 0.534(3) 0.040 Uiso 1 1 d D
C4 C 0.5058(3) 0.0770(3) 0.5135(3) 0.0267(6) Uani 1 1 d D
C5 C 0.3848(4) 0.1383(3) 0.5014(3) 0.0319(7) Uani 1 1 d D
H5A H 0.388(3) 0.227(2) 0.553(3) 0.038 Uiso 1 1 d D
H5B H 0.2850(19) 0.080(2) 0.472(3) 0.038 Uiso 1 1 d D
P1 P 0.30513(8) 0.14993(7) 0.20680(7) 0.02483(18) Uani 1 1 d .
C11 C 0.1542(3) 0.2226(3) 0.2371(3) 0.0303(7) Uani 1 1 d .
H11A H 0.0792 0.2095 0.1540 0.036 Uiso 1 1 calc R
H11B H 0.1112 0.1672 0.2998 0.036 Uiso 1 1 calc R
C12 C 0.1926(4) 0.3788(3) 0.2907(3) 0.0383(8) Uani 1 1 d .
H12A H 0.2526 0.3896 0.3814 0.046 Uiso 1 1 calc R
H12B H 0.2518 0.4327 0.2375 0.046 Uiso 1 1 calc R
C13 C 0.0620(4) 0.4428(4) 0.2911(4) 0.0574(10) Uani 1 1 d .
H13A H 0.0971 0.5408 0.3346 0.069 Uiso 1 1 calc R
H13B H 0.0124 0.4479 0.1993 0.069 Uiso 1 1 calc R
C14 C -0.0437(5) 0.3678(4) 0.3554(5) 0.0760(14) Uani 1 1 d .
H14A H -0.1240 0.4157 0.3486 0.114 Uiso 1 1 calc R
H14B H 0.0023 0.3664 0.4478 0.114 Uiso 1 1 calc R
H14C H -0.0804 0.2707 0.3130 0.114 Uiso 1 1 calc R
C21 C 0.3348(3) 0.2146(3) 0.0526(3) 0.0273(6) Uani 1 1 d .
H21A H 0.3739 0.3179 0.0702 0.033 Uiso 1 1 calc R
H21B H 0.4111 0.1723 0.0285 0.033 Uiso 1 1 calc R
C22 C 0.2078(3) 0.1880(3) -0.0663(3) 0.0309(7) Uani 1 1 d .
H22A H 0.1314 0.2326 -0.0455 0.037 Uiso 1 1 calc R
H22B H 0.1672 0.0851 -0.0860 0.037 Uiso 1 1 calc R
C23 C 0.2493(4) 0.2455(3) -0.1871(3) 0.0351(7) Uani 1 1 d .
H23A H 0.2844 0.3493 -0.1692 0.042 Uiso 1 1 calc R
H23B H 0.3295 0.2051 -0.2049 0.042 Uiso 1 1 calc R
C24 C 0.1235(4) 0.2109(4) -0.3073(3) 0.0516(9) Uani 1 1 d .
H24A H 0.1548 0.2509 -0.3819 0.077 Uiso 1 1 calc R
H24B H 0.0440 0.2513 -0.2904 0.077 Uiso 1 1 calc R
H24C H 0.0905 0.1082 -0.3272 0.077 Uiso 1 1 calc R
C31 C 0.2126(3) -0.0354(3) 0.1596(3) 0.0298(7) Uani 1 1 d .
H31A H 0.1801 -0.0732 0.2355 0.036 Uiso 1 1 calc R
H31B H 0.1251 -0.0399 0.0889 0.036 Uiso 1 1 calc R
C32 C 0.3013(3) -0.1316(3) 0.1129(3) 0.0284(7) Uani 1 1 d .
H32A H 0.3354 -0.0945 0.0374 0.034 Uiso 1 1 calc R
H32B H 0.3874 -0.1310 0.1839 0.034 Uiso 1 1 calc R
C33 C 0.2145(3) -0.2826(3) 0.0728(3) 0.0370(8) Uani 1 1 d .
H33A H 0.1821 -0.3194 0.1491 0.044 Uiso 1 1 calc R
H33B H 0.1270 -0.2820 0.0037 0.044 Uiso 1 1 calc R
C34 C 0.2968(4) -0.3819(3) 0.0226(4) 0.0481(9) Uani 1 1 d .
H34A H 0.2359 -0.4776 0.0028 0.072 Uiso 1 1 calc R
H34B H 0.3848 -0.3819 0.0895 0.072 Uiso 1 1 calc R
H34C H 0.3232 -0.3504 -0.0570 0.072 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'
O O 0.0106 0.0060 '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'
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
C2 Co1 C1 110.52(12) . .
C2 Co1 C4 103.27(12) . .
C1 Co1 C4 127.93(11) . .
C2 Co1 C3 93.75(13) . .
C1 Co1 C3 97.31(13) . .
C4 Co1 C3 41.06(11) . .
C2 Co1 C5 138.75(12) . .
C1 Co1 C5 108.88(12) . .
C4 Co1 C5 39.95(12) . .
C3 Co1 C5 69.45(13) . .
C2 Co1 P1 94.71(10) . .
C1 Co1 P1 99.07(10) . .
C4 Co1 P1 116.62(9) . .
C3 Co1 P1 157.60(9) . .
C5 Co1 P1 90.75(10) . .
O1 C1 Co1 173.4(3) . .
O2 C2 Co1 177.9(3) . .
C4 C3 Co1 68.34(17) . .
C4 C3 H3A 118.3(14) . .
Co1 C3 H3A 108.4(18) . .
C4 C3 H3B 121.1(14) . .
Co1 C3 H3B 117.1(18) . .
H3A C3 H3B 114(2) . .
C5 C4 C3 112.8(3) . .
C5 C4 C4 123.2(3) . 2_656
C3 C4 C4 123.5(3) . 2_656
C5 C4 Co1 72.87(16) . .
C3 C4 Co1 70.60(16) . .
C4 C4 Co1 118.1(2) 2_656 .
C4 C5 Co1 67.18(16) . .
C4 C5 H5A 122.5(15) . .
Co1 C5 H5A 105.7(17) . .
C4 C5 H5B 121.4(14) . .
Co1 C5 H5B 119.4(17) . .
H5A C5 H5B 112(2) . .
C31 P1 C11 99.65(13) . .
C31 P1 C21 104.10(12) . .
C11 P1 C21 104.58(13) . .
C31 P1 Co1 117.22(11) . .
C11 P1 Co1 117.14(9) . .
C21 P1 Co1 112.34(10) . .
C12 C11 P1 115.6(2) . .
C12 C11 H11A 108.4 . .
P1 C11 H11A 108.4 . .
C12 C11 H11B 108.4 . .
P1 C11 H11B 108.4 . .
H11A C11 H11B 107.5 . .
C13 C12 C11 114.2(3) . .
C13 C12 H12A 108.7 . .
C11 C12 H12A 108.7 . .
C13 C12 H12B 108.7 . .
C11 C12 H12B 108.7 . .
H12A C12 H12B 107.6 . .
C14 C13 C12 115.7(3) . .
C14 C13 H13A 108.3 . .
C12 C13 H13A 108.3 . .
C14 C13 H13B 108.3 . .
C12 C13 H13B 108.3 . .
H13A C13 H13B 107.4 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C22 C21 P1 118.79(19) . .
C22 C21 H21A 107.6 . .
P1 C21 H21A 107.6 . .
C22 C21 H21B 107.6 . .
P1 C21 H21B 107.6 . .
H21A C21 H21B 107.0 . .
C21 C22 C23 112.8(2) . .
C21 C22 H22A 109.0 . .
C23 C22 H22A 109.0 . .
C21 C22 H22B 109.0 . .
C23 C22 H22B 109.0 . .
H22A C22 H22B 107.8 . .
C24 C23 C22 112.4(3) . .
C24 C23 H23A 109.1 . .
C22 C23 H23A 109.1 . .
C24 C23 H23B 109.1 . .
C22 C23 H23B 109.1 . .
H23A C23 H23B 107.9 . .
C23 C24 H24A 109.5 . .
C23 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C23 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C32 C31 P1 115.8(2) . .
C32 C31 H31A 108.3 . .
P1 C31 H31A 108.3 . .
C32 C31 H31B 108.3 . .
P1 C31 H31B 108.3 . .
H31A C31 H31B 107.4 . .
C33 C32 C31 112.1(2) . .
C33 C32 H32A 109.2 . .
C31 C32 H32A 109.2 . .
C33 C32 H32B 109.2 . .
C31 C32 H32B 109.2 . .
H32A C32 H32B 107.9 . .
C34 C33 C32 114.1(3) . .
C34 C33 H33A 108.7 . .
C32 C33 H33A 108.7 . .
C34 C33 H33B 108.7 . .
C32 C33 H33B 108.7 . .
H33A C33 H33B 107.6 . .
C33 C34 H34A 109.5 . .
C33 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C33 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 C2 1.747(3) .
Co1 C1 1.773(3) .
Co1 C4 2.023(3) .
Co1 C3 2.054(3) .
Co1 C5 2.098(3) .
Co1 P1 2.1811(9) .
O1 C1 1.158(3) .
O2 C2 1.162(3) .
C3 C4 1.430(4) .
C3 H3A 0.999(18) .
C3 H3B 0.981(17) .
C4 C5 1.410(4) .
C4 C4 1.484(5) 2_656
C5 H5A 0.984(17) .
C5 H5B 0.990(17) .
P1 C31 1.829(3) .
P1 C11 1.833(3) .
P1 C21 1.841(3) .
C11 C12 1.530(4) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.525(5) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.455(5) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C21 C22 1.518(4) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 C23 1.526(4) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C24 1.520(4) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C31 C32 1.524(4) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
C32 C33 1.521(3) .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C33 C34 1.516(4) .
C33 H33A 0.9900 .
C33 H33B 0.9900 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 Co1 C3 C4 -105.97(18) . .
C1 Co1 C3 C4 142.77(18) . .
C5 Co1 C3 C4 35.30(16) . .
P1 Co1 C3 C4 6.0(3) . .
Co1 C3 C4 C5 -60.9(2) . .
Co1 C3 C4 C4 111.5(3) . 2_656
C2 Co1 C4 C5 -157.13(18) . .
C1 Co1 C4 C5 73.0(2) . .
C3 Co1 C4 C5 122.6(2) . .
P1 Co1 C4 C5 -54.86(17) . .
C2 Co1 C4 C3 80.30(19) . .
C1 Co1 C4 C3 -49.5(2) . .
C5 Co1 C4 C3 -122.6(2) . .
P1 Co1 C4 C3 -177.43(14) . .
C2 Co1 C4 C4 -38.1(3) . 2_656
C1 Co1 C4 C4 -167.9(3) . 2_656
C3 Co1 C4 C4 -118.4(4) . 2_656
C5 Co1 C4 C4 119.1(4) . 2_656
P1 Co1 C4 C4 64.2(3) . 2_656
C3 C4 C5 Co1 59.6(2) . .
C4 C4 C5 Co1 -112.8(3) 2_656 .
C2 Co1 C5 C4 35.0(3) . .
C1 Co1 C5 C4 -127.12(18) . .
C3 Co1 C5 C4 -36.24(16) . .
P1 Co1 C5 C4 133.02(15) . .
C2 Co1 P1 C31 68.21(13) . .
C1 Co1 P1 C31 179.88(13) . .
C4 Co1 P1 C31 -39.19(14) . .
C3 Co1 P1 C31 -43.6(3) . .
C5 Co1 P1 C31 -70.87(13) . .
C2 Co1 P1 C11 -173.40(13) . .
C1 Co1 P1 C11 -61.72(14) . .
C4 Co1 P1 C11 79.20(14) . .
C3 Co1 P1 C11 74.8(3) . .
C5 Co1 P1 C11 47.53(13) . .
C2 Co1 P1 C21 -52.30(13) . .
C1 Co1 P1 C21 59.37(13) . .
C4 Co1 P1 C21 -159.70(13) . .
C3 Co1 P1 C21 -164.1(3) . .
C5 Co1 P1 C21 168.62(12) . .
C31 P1 C11 C12 175.3(2) . .
C21 P1 C11 C12 -77.2(2) . .
Co1 P1 C11 C12 47.8(2) . .
P1 C11 C12 C13 169.3(2) . .
C11 C12 C13 C14 53.0(4) . .
C31 P1 C21 C22 50.6(2) . .
C11 P1 C21 C22 -53.5(2) . .
Co1 P1 C21 C22 178.45(18) . .
P1 C21 C22 C23 -179.1(2) . .
C21 C22 C23 C24 176.7(3) . .
C11 P1 C31 C32 174.3(2) . .
C21 P1 C31 C32 66.5(2) . .
Co1 P1 C31 C32 -58.2(2) . .
P1 C31 C32 C33 -178.7(2) . .
C31 C32 C33 C34 178.7(3) . .
