#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/43/2014324.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2014324
loop_
_publ_author_name
'Jonathan C. Burley'
'Timothy J. Prior'
_publ_section_title
;
 Insights into crystallization mechanism: a synchrotron study of
 polymorphism in a cobalt acetate cluster compound
;
_journal_coeditor_code           FA1176
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m63
_journal_page_last               m66
_journal_paper_doi               10.1107/S0108270105041570
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Co3 (C2 H3 O2)4 (C5 H5 N)8] (P F6)2'
_chemical_formula_moiety         'C48 H52 Co3 N8 O8 2+ , 2F6 P -'
_chemical_formula_sum            'C48 H52 Co3 F12 N8 O8 P2'
_chemical_formula_weight         1335.71
_chemical_name_common
;
di-μ₃-acetato-1κ²O,O':2\kO';2\kO:3κ²O,O'-di-μ₂-acetato-
1\kO:2\kO';2\kO:3\kO'-octapyridyl-1κ³N,2κ²N,3κ³N-tricobalt(II)
bis(hexafluorophosphate)
;
_chemical_name_systematic
;
  ?
;
_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
_audit_creation_method           SHELXL97
_cell_angle_alpha                98.149(5)
_cell_angle_beta                 103.605(5)
_cell_angle_gamma                111.722(5)
_cell_formula_units_Z            1
_cell_length_a                   10.688(4)
_cell_length_b                   11.839(4)
_cell_length_c                   12.480(4)
_cell_measurement_reflns_used    3499
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.99
_cell_volume                     1379.3(8)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        APEX2
_computing_molecular_graphics
'WinGX (Version 1.64; Farrugia, 1999) and PLATON (Spek, 2003)'
_computing_publication_material  SHEXLX97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67110
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11698
_diffrn_reflns_theta_full        24.80
_diffrn_reflns_theta_max         24.80
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             679
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.292
_refine_diff_density_min         -0.835
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0723
_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)+(0.1413P)²+0.0662P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.2144
_reflns_number_gt                3897
_reflns_number_total             5565
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fa1176.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2014324
_cod_database_fobs_code          2014324
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Co1 0.0000 0.0000 0.0000 0.0251(3) Uani d S 1 . . Co
O1 -0.0951(4) 0.1167(3) 0.0320(3) 0.0316(8) Uani d . 1 . . O
O2 0.0088(4) 0.3256(3) 0.0552(3) 0.0371(9) Uani d . 1 . . O
C1 -0.0998(6) 0.2202(5) 0.0310(4) 0.0314(11) Uani d . 1 . . C
C2 -0.2417(6) 0.2246(6) 0.0035(5) 0.0418(13) Uani d . 1 . . C
H2A -0.3048 0.1624 -0.0683 0.063 Uiso calc R 1 . . H
H2B -0.2308 0.3087 -0.0041 0.063 Uiso calc R 1 . . H
H2C -0.2824 0.2055 0.0649 0.063 Uiso calc R 1 . . H
Co2 0.21063(7) 0.35336(6) 0.07863(6) 0.0318(2) Uani d . 1 . . Co
O3 0.1867(4) 0.1623(3) 0.0132(3) 0.0311(8) Uani d . 1 . . O
O4 0.3916(4) 0.3243(3) 0.0648(3) 0.0356(8) Uani d . 1 . . O
C3 0.3190(5) 0.2063(5) 0.0248(4) 0.0313(11) Uani d . 1 . . C
C4 0.3864(6) 0.1229(5) -0.0078(5) 0.0369(12) Uani d . 1 . . C
H4A 0.3133 0.0372 -0.0436 0.055 Uiso calc R 1 . . H
H4B 0.4544 0.1230 0.0603 0.055 Uiso calc R 1 . . H
H4C 0.4359 0.1536 -0.0618 0.055 Uiso calc R 1 . . H
N1 0.0725(4) 0.0084(4) 0.1758(4) 0.0297(9) Uani d . 1 . . N
C10 -0.0119(6) 0.0034(6) 0.2405(5) 0.0398(13) Uani d . 1 . . C
H10 -0.1013 0.0044 0.2084 0.048 Uiso calc R 1 . . H
C11 0.0264(7) -0.0031(7) 0.3525(5) 0.0539(17) Uani d . 1 . . C
H11 -0.0374 -0.0086 0.3953 0.065 Uiso calc R 1 . . H
C12 0.1550(7) -0.0015(7) 0.4014(5) 0.0493(16) Uani d . 1 . . C
H12 0.1820 -0.0067 0.4781 0.059 Uiso calc R 1 . . H
C13 0.2456(6) 0.0077(5) 0.3370(5) 0.0374(12) Uani d . 1 . . C
H13 0.3371 0.0106 0.3689 0.045 Uiso calc R 1 . . H
C14 0.2003(5) 0.0124(5) 0.2257(4) 0.0299(11) Uani d . 1 . . C
H14 0.2630 0.0189 0.1818 0.036 Uiso calc R 1 . . H
N2 0.1892(5) 0.3914(4) -0.0887(4) 0.0338(10) Uani d . 1 . . N
C20 0.2854(6) 0.4924(5) -0.1048(5) 0.0375(12) Uani d . 1 . . C
H20 0.3695 0.5428 -0.0432 0.045 Uiso calc R 1 . . H
C21 0.2687(7) 0.5273(5) -0.2069(5) 0.0409(13) Uani d . 1 . . C
H21 0.3398 0.6001 -0.2147 0.049 Uiso calc R 1 . . H
C22 0.1481(7) 0.4553(6) -0.2962(5) 0.0450(14) Uani d . 1 . . C
H22 0.1324 0.4783 -0.3664 0.054 Uiso calc R 1 . . H
C23 0.0502(7) 0.3487(7) -0.2819(5) 0.0567(18) Uani d . 1 . . C
H23 -0.0328 0.2950 -0.3432 0.068 Uiso calc R 1 . . H
C24 0.0739(7) 0.3211(6) -0.1784(5) 0.0495(16) Uani d . 1 . . C
H24 0.0046 0.2479 -0.1695 0.059 Uiso calc R 1 . . H
N3 0.3173(5) 0.5473(4) 0.1667(4) 0.0371(10) Uani d . 1 . . N
C30 0.4553(7) 0.6139(5) 0.1883(5) 0.0413(13) Uani d . 1 . . C
H30 0.5053 0.5776 0.1521 0.050 Uiso calc R 1 . . H
C31 0.5305(7) 0.7337(6) 0.2608(5) 0.0491(16) Uani d . 1 . . C
H31 0.6286 0.7794 0.2715 0.059 Uiso calc R 1 . . H
C32 0.4595(8) 0.7850(6) 0.3171(6) 0.0509(16) Uani d . 1 . . C
H32 0.5086 0.8655 0.3695 0.061 Uiso calc R 1 . . H
C33 0.3181(8) 0.7184(6) 0.2963(6) 0.0566(17) Uani d . 1 . . C
H33 0.2668 0.7520 0.3335 0.068 Uiso calc R 1 . . H
C34 0.2496(7) 0.6006(6) 0.2202(6) 0.0498(15) Uani d . 1 . . C
H34 0.1504 0.5556 0.2051 0.060 Uiso calc R 1 . . H
N4 0.2392(5) 0.3279(4) 0.2510(4) 0.0401(11) Uani d . 1 . . N
C40 0.3638(7) 0.3365(5) 0.3152(5) 0.0451(14) Uani d . 1 . . C
H40 0.4333 0.3376 0.2794 0.054 Uiso calc R 1 . . H
C41 0.3959(8) 0.3436(7) 0.4293(6) 0.0555(17) Uani d . 1 . . C
H41 0.4855 0.3493 0.4712 0.067 Uiso calc R 1 . . H
C42 0.2966(9) 0.3426(7) 0.4829(6) 0.066(2) Uani d . 1 . . C
H42 0.3175 0.3505 0.5626 0.079 Uiso calc R 1 . . H
C43 0.1672(9) 0.3301(8) 0.4184(6) 0.070(2) Uani d . 1 . . C
H43 0.0952 0.3260 0.4521 0.084 Uiso calc R 1 . . H
C44 0.1434(7) 0.3235(6) 0.3042(5) 0.0521(16) Uani d . 1 . . C
H44 0.0534 0.3155 0.2604 0.063 Uiso calc R 1 . . H
P1 0.69698(16) 0.16469(15) 0.35473(13) 0.0398(4) Uani d . 1 . . P
F1 0.6597(7) 0.2811(5) 0.3789(5) 0.0922(17) Uani d . 1 . . F
F2 0.5529(5) 0.0923(6) 0.2524(4) 0.0865(16) Uani d . 1 . . F
F3 0.7788(5) 0.2235(4) 0.2704(4) 0.0707(12) Uani d . 1 . . F
F4 0.7324(4) 0.0456(4) 0.3302(3) 0.0585(10) Uani d . 1 . . F
F5 0.8387(5) 0.2319(4) 0.4577(3) 0.0755(13) Uani d . 1 . . F
F6 0.6166(4) 0.1054(3) 0.4400(3) 0.0474(8) Uani d . 1 . . F
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'
O O 0.0106 0.0060 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Co1 O1 . 2 180.0(2)
O1 Co1 N1 . 2 88.44(15)
O1 Co1 N1 2 2 91.56(15)
O1 Co1 N1 . . 91.56(15)
O1 Co1 N1 2 . 88.44(15)
N1 Co1 N1 2 . 180.00(8)
O1 Co1 O3 . . 88.62(14)
O1 Co1 O3 2 . 91.38(14)
N1 Co1 O3 2 . 87.68(14)
N1 Co1 O3 . . 92.32(14)
O1 Co1 O3 . 2 91.38(14)
O1 Co1 O3 2 2 88.62(14)
N1 Co1 O3 2 2 92.32(14)
N1 Co1 O3 . 2 87.68(14)
O3 Co1 O3 . 2 180.0(3)
C1 O1 Co1 . . 148.0(3)
C1 O2 Co2 . . 127.5(3)
O1 C1 O2 . . 125.1(5)
O1 C1 C2 . . 118.3(5)
O2 C1 C2 . . 116.6(5)
C1 C2 H2A . . 109.5
C1 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
C1 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
O2 Co2 O4 . . 161.20(15)
O2 Co2 N3 . . 100.56(17)
O4 Co2 N3 . . 97.84(17)
O2 Co2 N2 . . 88.23(16)
O4 Co2 N2 . . 86.76(15)
N3 Co2 N2 . . 93.59(17)
O2 Co2 N4 . . 92.53(17)
O4 Co2 N4 . . 93.60(17)
N3 Co2 N4 . . 82.83(17)
N2 Co2 N4 . . 176.41(17)
O2 Co2 O3 . . 101.43(14)
O4 Co2 O3 . . 60.72(13)
N3 Co2 O3 . . 157.39(16)
N2 Co2 O3 . . 92.30(15)
N4 Co2 O3 . . 90.99(15)
C3 O3 Co1 . . 146.3(3)
C3 O3 Co2 . . 89.3(3)
Co1 O3 Co2 . . 121.64(16)
C3 O4 Co2 . . 92.2(3)
O4 C3 O3 . . 117.8(5)
O4 C3 C4 . . 120.9(5)
O3 C3 C4 . . 121.3(5)
C3 C4 H4A . . 109.5
C3 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C3 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
C10 N1 C14 . . 117.0(5)
C10 N1 Co1 . . 120.5(4)
C14 N1 Co1 . . 122.4(3)
N1 C10 C11 . . 122.3(5)
N1 C10 H10 . . 118.9
C11 C10 H10 . . 118.9
C12 C11 C10 . . 120.1(6)
C12 C11 H11 . . 119.9
C10 C11 H11 . . 119.9
C11 C12 C13 . . 118.5(6)
C11 C12 H12 . . 120.8
C13 C12 H12 . . 120.8
C14 C13 C12 . . 118.4(5)
C14 C13 H13 . . 120.8
C12 C13 H13 . . 120.8
N1 C14 C13 . . 123.7(5)
N1 C14 H14 . . 118.1
C13 C14 H14 . . 118.1
C20 N2 C24 . . 116.6(5)
C20 N2 Co2 . . 121.4(4)
C24 N2 Co2 . . 121.9(4)
N2 C20 C21 . . 123.2(6)
N2 C20 H20 . . 118.4
C21 C20 H20 . . 118.4
C22 C21 C20 . . 118.9(5)
C22 C21 H21 . . 120.6
C20 C21 H21 . . 120.6
C21 C22 C23 . . 118.4(6)
C21 C22 H22 . . 120.8
C23 C22 H22 . . 120.8
C24 C23 C22 . . 119.2(6)
C24 C23 H23 . . 120.4
C22 C23 H23 . . 120.4
N2 C24 C23 . . 123.7(6)
N2 C24 H24 . . 118.2
C23 C24 H24 . . 118.2
C30 N3 C34 . . 116.9(5)
C30 N3 Co2 . . 122.9(4)
C34 N3 Co2 . . 119.2(4)
N3 C30 C31 . . 123.5(6)
N3 C30 H30 . . 118.2
C31 C30 H30 . . 118.2
C32 C31 C30 . . 118.5(6)
C32 C31 H31 . . 120.8
C30 C31 H31 . . 120.8
C33 C32 C31 . . 118.9(6)
C33 C32 H32 . . 120.5
C31 C32 H32 . . 120.5
C32 C33 C34 . . 119.2(6)
C32 C33 H33 . . 120.4
C34 C33 H33 . . 120.4
N3 C34 C33 . . 123.0(6)
N3 C34 H34 . . 118.5
C33 C34 H34 . . 118.5
C44 N4 C40 . . 116.3(6)
C44 N4 Co2 . . 121.8(5)
C40 N4 Co2 . . 121.0(4)
N4 C40 C41 . . 123.4(6)
N4 C40 H40 . . 118.3
C41 C40 H40 . . 118.3
C40 C41 C42 . . 119.1(7)
C40 C41 H41 . . 120.4
C42 C41 H41 . . 120.4
C43 C42 C41 . . 118.4(7)
C43 C42 H42 . . 120.8
C41 C42 H42 . . 120.8
C42 C43 C44 . . 118.8(7)
C42 C43 H43 . . 120.6
C44 C43 H43 . . 120.6
N4 C44 C43 . . 123.9(7)
N4 C44 H44 . . 118.1
C43 C44 H44 . . 118.1
F5 P1 F1 . . 91.1(3)
F5 P1 F2 . . 177.9(3)
F1 P1 F2 . . 90.4(3)
F5 P1 F3 . . 90.4(3)
F1 P1 F3 . . 90.8(2)
F2 P1 F3 . . 91.0(3)
F5 P1 F4 . . 89.5(3)
F1 P1 F4 . . 179.2(3)
F2 P1 F4 . . 89.0(3)
F3 P1 F4 . . 89.8(2)
F5 P1 F6 . . 89.1(2)
F1 P1 F6 . . 89.7(2)
F2 P1 F6 . . 89.5(2)
F3 P1 F6 . . 179.3(2)
F4 P1 F6 . . 89.7(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O1 . 2.044(3) ?
Co1 N1 . 2.122(4) ?
Co1 O3 . 2.150(3) ?
O1 C1 . 1.246(6) ?
O2 C1 . 1.285(7) ?
O2 Co2 . 1.999(4) ?
C1 C2 . 1.496(7) ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
C2 H2C . 0.9800 ?
Co2 O4 . 2.126(4) ?
Co2 N3 . 2.130(5) ?
Co2 N2 . 2.176(5) ?
Co2 N4 . 2.181(5) ?
Co2 O3 . 2.190(4) ?
O3 C3 . 1.276(6) ?
O4 C3 . 1.273(6) ?
C3 C4 . 1.487(8) ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C4 H4C . 0.9800 ?
N1 C10 . 1.337(7) ?
N1 C14 . 1.341(6) ?
C10 C11 . 1.382(8) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.359(9) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.381(8) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.376(7) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
N2 C20 . 1.335(7) ?
N2 C24 . 1.338(8) ?
C20 C21 . 1.387(8) ?
C20 H20 . 0.9500 ?
C21 C22 . 1.368(9) ?
C21 H21 . 0.9500 ?
C22 C23 . 1.377(9) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.366(9) ?
C23 H23 . 0.9500 ?
C24 H24 . 0.9500 ?
N3 C30 . 1.328(8) ?
N3 C34 . 1.347(8) ?
C30 C31 . 1.389(8) ?
C30 H30 . 0.9500 ?
C31 C32 . 1.382(10) ?
C31 H31 . 0.9500 ?
C32 C33 . 1.360(10) ?
C32 H32 . 0.9500 ?
C33 C34 . 1.387(9) ?
C33 H33 . 0.9500 ?
C34 H34 . 0.9500 ?
N4 C44 . 1.335(8) ?
N4 C40 . 1.341(8) ?
C40 C41 . 1.367(9) ?
C40 H40 . 0.9500 ?
C41 C42 . 1.378(10) ?
C41 H41 . 0.9500 ?
C42 C43 . 1.368(11) ?
C42 H42 . 0.9500 ?
C43 C44 . 1.374(9) ?
C43 H43 . 0.9500 ?
C44 H44 . 0.9500 ?
P1 F5 . 1.575(4) ?
P1 F1 . 1.579(5) ?
P1 F2 . 1.589(5) ?
P1 F3 . 1.596(4) ?
P1 F4 . 1.598(4) ?
P1 F6 . 1.599(3) ?
