#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:47:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179394 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/91/4329139.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_4329139
loop_
_publ_author_name
'John S. Maass'
'Matthias Zeller'
'Tanya M. Breault'
'Bart M. Bartlett'
'Hiroshi Sakiyama'
'Rudy L. Luck'
_publ_contact_author_address
;
Department of Chemistry
Michigan Technological University
1400 Townsend Drive
Houghton, MI USA 49931
;
_publ_contact_author_email       rluck@mtu.edu
_publ_contact_author_fax         '(906)487 2061'
_publ_contact_author_name        'Luck, Rudy L.'
_publ_contact_author_phone       '(906)487 2309'
_publ_section_title
;
 Syntheses and Structures of Three Complexes of Formulas
 [L3Co(μ2-O2P(Bn)2)3CoL'][L"], Featuring Octahedral and Tetrahedral
 Cobalt(II) Geometries; Variable-Temperature Magnetic Susceptibility
 Measurement and Analysis on [(py)3Co(μ2-O2PBn2)3Co(py)][ClO4]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4903
_journal_page_last               4905
_journal_paper_doi               10.1021/ic3004799
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C62 H62 Co2 N4 O6 P3, Cl O4'
_chemical_formula_sum            'C62 H62 Cl Co2 N4 O10 P3'
_chemical_formula_weight         1269.38
_chemical_name_systematic
;
 1 at 291
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-23T16:17:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.785(3)
_cell_length_b                   13.785(3)
_cell_length_c                   57.28(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_measurement_wavelength     0.71073
_cell_volume                     9426(4)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled ω scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.019817
_diffrn_orient_matrix_UB_12      -0.046793
_diffrn_orient_matrix_UB_13      -0.014455
_diffrn_orient_matrix_UB_21      0.038751
_diffrn_orient_matrix_UB_22      0.069412
_diffrn_orient_matrix_UB_23      -0.009707
_diffrn_orient_matrix_UB_31      0.071615
_diffrn_orient_matrix_UB_32      -0.001526
_diffrn_orient_matrix_UB_33      0.001254
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            4198
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.07
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  166
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.8261
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   9
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       prism
_exptl_crystal_F_000             3948
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3691
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      0.97
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0539P)²+9.3540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                1947
_reflns_number_total             3691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004799_si_002_2.cif
_cod_data_source_block           jmcodi
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4329139
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.6667 0.3333 0.395611(14) 0.0524(3) Uani 1 3 d S . .
Co2 Co 0.6667 0.3333 0.469773(16) 0.0687(4) Uani 1 3 d S . .
O1 O 0.5293(2) 0.2220(2) 0.41625(4) 0.0648(8) Uani 1 1 d . A .
O2 O 0.5128(2) 0.2333(2) 0.46063(4) 0.0689(8) Uani 1 1 d . A .
P1 P 0.45860(10) 0.21666(10) 0.436673(17) 0.0610(3) Uani 1 1 d . . .
C1 C 0.4140(4) 0.3192(4) 0.43319(7) 0.0711(13) Uani 1 1 d . A .
H1A H 0.4797 0.3927 0.4313 0.085 Uiso 1 1 calc R . .
H1B H 0.3698 0.3024 0.419 0.085 Uiso 1 1 calc R . .
C2 C 0.3461(5) 0.3224(4) 0.45338(8) 0.0732(13) Uani 1 1 d . . .
C3 C 0.3960(5) 0.3735(4) 0.47413(9) 0.0867(15) Uani 1 1 d . A .
H3 H 0.4736 0.4101 0.4753 0.104 Uiso 1 1 calc R . .
C4 C 0.3339(6) 0.3718(5) 0.49320(9) 0.0962(17) Uani 1 1 d . . .
H4 H 0.3702 0.4076 0.5069 0.115 Uiso 1 1 calc R A .
C5 C 0.2202(6) 0.3182(6) 0.49210(10) 0.118(2) Uani 1 1 d . A .
H5 H 0.1787 0.3175 0.505 0.142 Uiso 1 1 calc R . .
C6 C 0.1676(6) 0.2655(7) 0.47186(12) 0.140(3) Uani 1 1 d . . .
H6 H 0.0898 0.2271 0.4711 0.169 Uiso 1 1 calc R A .
C7 C 0.2303(6) 0.2692(6) 0.45246(9) 0.117(2) Uani 1 1 d . A .
H7 H 0.1937 0.2354 0.4386 0.14 Uiso 1 1 calc R . .
C8 C 0.3343(4) 0.0797(4) 0.43833(7) 0.0705(13) Uani 1 1 d . A .
H8A H 0.354 0.0302 0.4464 0.085 Uiso 1 1 calc R . .
H8B H 0.2798 0.0862 0.4479 0.085 Uiso 1 1 calc R . .
C9 C 0.2781(4) 0.0241(4) 0.41571(8) 0.0646(12) Uani 1 1 d . . .
C10 C 0.2213(5) 0.0613(5) 0.40215(10) 0.0974(17) Uani 1 1 d . A .
H10 H 0.2145 0.1218 0.4072 0.117 Uiso 1 1 calc R . .
C11 C 0.1737(5) 0.0106(6) 0.38104(12) 0.120(2) Uani 1 1 d . . .
H11 H 0.1377 0.0391 0.372 0.144 Uiso 1 1 calc R A .
C12 C 0.1786(6) -0.0780(6) 0.37352(11) 0.111(2) Uani 1 1 d . A .
H12 H 0.1444 -0.1127 0.3596 0.133 Uiso 1 1 calc R . .
C13 C 0.2341(5) -0.1174(5) 0.38645(12) 0.1068(19) Uani 1 1 d . . .
H13 H 0.2387 -0.179 0.3813 0.128 Uiso 1 1 calc R A .
C14 C 0.2842(4) -0.0657(5) 0.40742(10) 0.0907(16) Uani 1 1 d . A .
H14 H 0.3228 -0.0929 0.416 0.109 Uiso 1 1 calc R . .
N1 N 0.8136(3) 0.4546(3) 0.37525(5) 0.0566(9) Uani 1 1 d . . .
C15 C 0.9129(4) 0.4635(4) 0.37852(7) 0.0669(12) Uani 1 1 d . . .
H15 H 0.9166 0.4102 0.3879 0.08 Uiso 1 1 calc R . .
C16 C 1.0102(4) 0.5462(5) 0.36898(9) 0.0818(14) Uani 1 1 d . . .
H16 H 1.0777 0.5486 0.372 0.098 Uiso 1 1 calc R . .
C17 C 1.0077(5) 0.6247(5) 0.35512(9) 0.0890(16) Uani 1 1 d . . .
H17 H 1.0727 0.681 0.3482 0.107 Uiso 1 1 calc R . .
C18 C 0.9077(5) 0.6188(4) 0.35158(9) 0.0932(17) Uani 1 1 d . . .
H18 H 0.9033 0.6721 0.3424 0.112 Uiso 1 1 calc R . .
C19 C 0.8123(4) 0.5332(4) 0.36166(8) 0.0766(14) Uani 1 1 d . . .
H19 H 0.7442 0.5299 0.3589 0.092 Uiso 1 1 calc R . .
N2 N 0.654(15) 0.347(14) 0.50546(15) 0.037(6) Uani 0.33 1 d P A -1
C20 C 0.578(4) 0.293(5) 0.5164(6) 0.120(19) Uani 0.33 1 d PU A -1
H20 H 0.5196 0.2352 0.5083 0.144 Uiso 0.33 1 calc PR A -1
C21 C 0.5560(19) 0.297(3) 0.5406(4) 0.110(9) Uani 0.33 1 d PU A -1
H21 H 0.4863 0.2807 0.5462 0.132 Uiso 0.33 1 calc PR A -1
C22 C 0.638(3) 0.323(10) 0.5533(3) 0.106(11) Uani 0.33 1 d PU A -1
H22 H 0.6292 0.304 0.5691 0.127 Uiso 0.33 1 calc PR A -1
C23 C 0.750(2) 0.386(4) 0.5425(4) 0.126(12) Uani 0.33 1 d PU A -1
H23 H 0.8141 0.4107 0.5515 0.151 Uiso 0.33 1 calc PR A -1
C24 C 0.758(3) 0.408(7) 0.5184(5) 0.119(14) Uani 0.33 1 d PU A -1
H24 H 0.8256 0.4572 0.5112 0.143 Uiso 0.33 1 calc PR A -1
Cl1 Cl 0.3333 0.6667 0.34958(4) 0.0741(6) Uani 1 3 d S . .
O3 O 0.4392(3) 0.6900(4) 0.34140(7) 0.1209(14) Uani 1 1 d . . .
O4 O 0.3333 0.6667 0.37424(11) 0.126(3) Uani 1 3 d S . .
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 0 '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'
O O 0.0106 0.006 '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'
Cl Cl 0.1484 0.1585 '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_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 0 -26
3 -3 27
3 0 -27
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
O1 Co1 O1 91.55(10) 2_655 .
O1 Co1 O1 91.55(10) 2_655 3_665
O1 Co1 O1 91.55(10) . 3_665
O1 Co1 N1 87.42(12) 2_655 .
O1 Co1 N1 177.62(11) . .
O1 Co1 N1 86.33(12) 3_665 .
O1 Co1 N1 177.62(11) 2_655 2_655
O1 Co1 N1 86.33(12) . 2_655
O1 Co1 N1 87.43(12) 3_665 2_655
N1 Co1 N1 94.65(11) . 2_655
O1 Co1 N1 86.33(11) 2_655 3_665
O1 Co1 N1 87.43(12) . 3_665
O1 Co1 N1 177.62(11) 3_665 3_665
N1 Co1 N1 94.65(11) . 3_665
N1 Co1 N1 94.65(11) 2_655 3_665
O2 Co2 O2 112.97(6) . 3_665
O2 Co2 O2 112.97(6) . 2_655
O2 Co2 O2 112.97(6) 3_665 2_655
O2 Co2 N2 103(5) . .
O2 Co2 N2 100(4) 3_665 .
O2 Co2 N2 114.4(13) 2_655 .
O2 Co2 N2 100(4) . 2_655
O2 Co2 N2 114.4(14) 3_665 2_655
O2 Co2 N2 103(5) 2_655 2_655
N2 Co2 N2 15.4(9) . 2_655
O2 Co2 N2 114.4(14) . 3_665
O2 Co2 N2 103(5) 3_665 3_665
O2 Co2 N2 100(4) 2_655 3_665
N2 Co2 N2 15.4(9) . 3_665
N2 Co2 N2 15.4(9) 2_655 3_665
P1 O1 Co1 143.05(18) . .
P1 O2 Co2 129.09(16) . .
O1 P1 O2 115.93(17) . .
O1 P1 C8 110.19(19) . .
O2 P1 C8 104.30(19) . .
O1 P1 C1 109.92(18) . .
O2 P1 C1 108.29(19) . .
C8 P1 C1 107.8(2) . .
C2 C1 P1 113.4(3) . .
C2 C1 H1A 108.9 . .
P1 C1 H1A 108.9 . .
C2 C1 H1B 108.9 . .
P1 C1 H1B 108.9 . .
H1A C1 H1B 107.7 . .
C3 C2 C7 116.9(5) . .
C3 C2 C1 121.3(5) . .
C7 C2 C1 121.7(5) . .
C2 C3 C4 121.8(6) . .
C2 C3 H3 119.1 . .
C4 C3 H3 119.1 . .
C5 C4 C3 120.6(5) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
C4 C5 C6 119.3(6) . .
C4 C5 H5 120.4 . .
C6 C5 H5 120.4 . .
C5 C6 C7 120.2(6) . .
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 . .
C2 C7 C6 121.2(5) . .
C2 C7 H7 119.4 . .
C6 C7 H7 119.4 . .
C9 C8 P1 117.6(3) . .
C9 C8 H8A 107.9 . .
P1 C8 H8A 107.9 . .
C9 C8 H8B 107.9 . .
P1 C8 H8B 107.9 . .
H8A C8 H8B 107.2 . .
C14 C9 C10 116.6(5) . .
C14 C9 C8 120.7(5) . .
C10 C9 C8 122.7(5) . .
C9 C10 C11 121.3(6) . .
C9 C10 H10 119.4 . .
C11 C10 H10 119.4 . .
C12 C11 C10 121.2(6) . .
C12 C11 H11 119.4 . .
C10 C11 H11 119.4 . .
C11 C12 C13 119.2(6) . .
C11 C12 H12 120.4 . .
C13 C12 H12 120.4 . .
C12 C13 C14 120.0(6) . .
C12 C13 H13 120 . .
C14 C13 H13 120 . .
C9 C14 C13 121.6(6) . .
C9 C14 H14 119.2 . .
C13 C14 H14 119.2 . .
C15 N1 C19 115.9(4) . .
C15 N1 Co1 120.6(3) . .
C19 N1 Co1 122.8(3) . .
N1 C15 C16 123.9(5) . .
N1 C15 H15 118 . .
C16 C15 H15 118 . .
C17 C16 C15 119.6(5) . .
C17 C16 H16 120.2 . .
C15 C16 H16 120.2 . .
C18 C17 C16 118.1(5) . .
C18 C17 H17 121 . .
C16 C17 H17 121 . .
C17 C18 C19 119.7(5) . .
C17 C18 H18 120.2 . .
C19 C18 H18 120.2 . .
N1 C19 C18 122.8(5) . .
N1 C19 H19 118.6 . .
C18 C19 H19 118.6 . .
C20 N2 C24 114.7(17) . .
C20 N2 Co2 126(10) . .
C24 N2 Co2 117(8) . .
N2 C20 C21 132(7) . .
N2 C20 H20 114.1 . .
C21 C20 H20 114.1 . .
C22 C21 C20 114(3) . .
C22 C21 H21 123.1 . .
C20 C21 H21 123.1 . .
C21 C22 C23 117(3) . .
C21 C22 H22 121.4 . .
C23 C22 H22 121.4 . .
C24 C23 C22 119(3) . .
C24 C23 H23 120.4 . .
C22 C23 H23 120.4 . .
C23 C24 N2 115(6) . .
C23 C24 H24 122.3 . .
N2 C24 H24 122.3 . .
O3 Cl1 O3 109.50(18) 3_565 2_665
O3 Cl1 O3 109.50(18) 3_565 .
O3 Cl1 O3 109.50(18) 2_665 .
O3 Cl1 O4 109.45(18) 3_565 .
O3 Cl1 O4 109.45(18) 2_665 .
O3 Cl1 O4 109.45(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.105(3) 2_655
Co1 O1 2.105(3) .
Co1 O1 2.106(3) 3_665
Co1 N1 2.207(3) .
Co1 N1 2.207(3) 2_655
Co1 N1 2.207(3) 3_665
Co2 O2 1.937(3) .
Co2 O2 1.937(3) 3_665
Co2 O2 1.937(3) 2_655
Co2 N2 2.069(10) .
Co2 N2 2.069(10) 2_655
Co2 N2 2.069(10) 3_665
O1 P1 1.500(3) .
O2 P1 1.524(3) .
P1 C8 1.809(5) .
P1 C1 1.812(5) .
C1 C2 1.503(6) .
C1 H1A 0.97 .
C1 H1B 0.97 .
C2 C3 1.377(6) .
C2 C7 1.385(7) .
C3 C4 1.381(7) .
C3 H3 0.93 .
C4 C5 1.360(8) .
C4 H4 0.93 .
C5 C6 1.368(8) .
C5 H5 0.93 .
C6 C7 1.393(8) .
C6 H6 0.93 .
C7 H7 0.93 .
C8 C9 1.508(6) .
C8 H8A 0.97 .
C8 H8B 0.97 .
C9 C14 1.367(7) .
C9 C10 1.373(6) .
C10 C11 1.387(7) .
C10 H10 0.93 .
C11 C12 1.328(8) .
C11 H11 0.93 .
C12 C13 1.358(8) .
C12 H12 0.93 .
C13 C14 1.391(7) .
C13 H13 0.93 .
C14 H14 0.93 .
N1 C15 1.326(5) .
N1 C19 1.341(5) .
C15 C16 1.367(6) .
C15 H15 0.93 .
C16 C17 1.357(7) .
C16 H16 0.93 .
C17 C18 1.356(7) .
C17 H17 0.93 .
C18 C19 1.379(6) .
C18 H18 0.93 .
C19 H19 0.93 .
N2 C20 1.12(17) .
N2 C24 1.45(17) .
C20 C21 1.42(4) .
C20 H20 0.93 .
C21 C22 1.24(3) .
C21 H21 0.93 .
C22 C23 1.48(5) .
C22 H22 0.93 .
C23 C24 1.40(4) .
C23 H23 0.93 .
C24 H24 0.93 .
Cl1 O3 1.408(4) 3_565
Cl1 O3 1.408(4) 2_665
Cl1 O3 1.408(4) .
Cl1 O4 1.412(6) .
