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#$Date: 2016-03-25 13:37:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179854 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/50/7015091.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_7015091
loop_
_publ_author_name
'Keene, Tony D.'
'Light, Mark E.'
'Hursthouse, Michael B.'
'Price, Daniel J.'
_publ_section_title
;
 Structure and magnetism of new hybrid cobalt hydroxide materials built
 from decorated brucite layers.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2983
_journal_page_last               2994
_journal_paper_doi               10.1039/c0dt01007c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C5 H14 Co6 N O15'
_chemical_formula_sum            'C5 H14 Co6 N O15'
_chemical_formula_weight         681.75
_chemical_name_common
;Catena(octadecahydroxo-trioxalato-(mu -piperazine)-dodeca-
cobalt(ii))
;
_chemical_name_systematic
;
Catena(octadecahydroxo-trioxalato-(μ -piperazine)-dodeca-
cobalt(II))
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   9.420(2)
_cell_length_b                   9.420(2)
_cell_length_c                   10.242(4)
_cell_measurement_reflns_used    11764
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     787.1(4)
_computing_cell_refinement
'DENZO (Otwinowski and Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_collection       'DENZO (Otwinowski and Minor, 1997)'
_computing_data_reduction
'DENZO (Otwinowski and Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement
;SHELXS-97 (Sheldrick, 1997a) in WINGX (L.J. Farrugia, J. Appl. Cryst.,
1999, 32, 837-838
;
_computing_structure_solution
;SHELXS-97 (Sheldrick, 1997a) in WINGX (L.J. Farrugia, J. Appl. Cryst.,
1999, 32, 837-838
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Nonius Kappa CCD Area Detector'
_diffrn_measurement_method       'φ and ω scans to fill Ewald Sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2249
_diffrn_reflns_av_sigmaI/netI    0.1973
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3998
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    6.259
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.322
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         1180
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.2156
_refine_ls_R_factor_gt           0.1209
_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)+(0.1048P)²+15.3818P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2786
_refine_ls_wR_factor_ref         0.3334
_reflns_number_gt                567
_reflns_number_total             1180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01007c.txt
_cod_data_source_block           1
_cod_database_code               7015091
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.3358(2) 0.3348(2) 0.4962(2) 0.0279(7) Uani 1 1 d . . .
Co2 Co 0.6667 0.3333 0.5026(4) 0.0293(11) Uani 1 3 d S . .
Co3 Co 0.0000 0.0000 0.6625(4) 0.0245(10) Uani 1 3 d S . .
Co4 Co 0.3333 0.6667 1.0051(6) 0.086(2) Uani 1 3 d S . .
O1 O 0.2337(13) 0.1173(13) 0.6197(12) 0.033(3) Uiso 1 1 d . . .
H1 H 0.2942 0.1494 0.7024 0.040 Uiso 1 1 calc R . .
O2 O 0.2221(12) 0.4408(12) 0.5998(11) 0.029(3) Uiso 1 1 d . . .
H2 H 0.2242 0.4409 0.6955 0.035 Uiso 1 1 calc R . .
O3 O 0.5550(11) 0.4440(11) 0.6059(10) 0.022(2) Uiso 1 1 d . . .
H3 H 0.5523 0.4424 0.7016 0.027 Uiso 1 1 calc R . .
N1 N 0.0000 0.0000 0.8560(4) 0.093(12) Uiso 1 3 d SD . .
H4 H 0.0641 0.1100 0.8680 0.112 Uiso 0.3333 1 calc PR . .
C2A C 0.099(5) -0.051(7) 0.9321(5) 0.065(13) Uiso 0.3333 1 d PD . .
H5 H 0.1991 -0.0209 0.8848 0.078 Uiso 0.3333 1 calc PR . .
H6 H 0.0386 -0.1698 0.9400 0.078 Uiso 0.3333 1 calc PR . .
C2B C -0.142(3) -0.023(7) 0.9321(5) 0.065(13) Uiso 0.3333 1 d PD . .
H7 H -0.2190 -0.1397 0.9400 0.078 Uiso 0.3333 1 calc PR . .
H8 H -0.1964 0.0255 0.8848 0.078 Uiso 0.3333 1 calc PR . .
O4 O 0.354(2) 0.488(2) 0.8921(17) 0.082(4) Uiso 1 1 d . . .
O5 O 0.485(2) 0.354(2) 0.8866(17) 0.082(4) Uiso 1 1 d . . .
C1 C 0.457(3) 0.457(3) 0.9348(16) 0.082(4) Uiso 1 1 d 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'
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'
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
O2 Co1 O2 176.8(4) 5_556 . ?
O2 Co1 O3 99.4(4) 5_556 4_666 ?
O2 Co1 O3 83.8(4) . 4_666 ?
O2 Co1 O3 84.2(4) 5_556 . ?
O2 Co1 O3 96.2(4) . . ?
O3 Co1 O3 84.6(4) 4_666 . ?
O2 Co1 O1 96.4(4) 5_556 6_556 ?
O2 Co1 O1 83.3(4) . 6_556 ?
O3 Co1 O1 92.9(4) 4_666 6_556 ?
O3 Co1 O1 177.5(4) . 6_556 ?
O2 Co1 O1 83.2(4) 5_556 . ?
O2 Co1 O1 93.7(4) . . ?
O3 Co1 O1 174.5(4) 4_666 . ?
O3 Co1 O1 90.7(4) . . ?
O1 Co1 O1 91.7(6) 6_556 . ?
O3 Co2 O3 96.8(4) 3_665 2_655 ?
O3 Co2 O3 96.8(4) 3_665 . ?
O3 Co2 O3 96.8(4) 2_655 . ?
O3 Co2 O2 82.5(4) 3_665 6_656 ?
O3 Co2 O2 83.0(4) 2_655 6_656 ?
O3 Co2 O2 179.3(4) . 6_656 ?
O3 Co2 O2 179.3(4) 3_665 5_556 ?
O3 Co2 O2 82.5(4) 2_655 5_556 ?
O3 Co2 O2 83.0(4) . 5_556 ?
O2 Co2 O2 97.6(4) 6_656 5_556 ?
O3 Co2 O2 83.0(4) 3_665 4_666 ?
O3 Co2 O2 179.3(4) 2_655 4_666 ?
O3 Co2 O2 82.5(4) . 4_666 ?
O2 Co2 O2 97.6(4) 6_656 4_666 ?
O2 Co2 O2 97.6(4) 5_556 4_666 ?
O1 Co3 O1 115.1(3) 3 2 ?
O1 Co3 O1 115.1(3) 3 . ?
O1 Co3 O1 115.1(3) 2 . ?
O1 Co3 N1 102.9(4) 3 . ?
O1 Co3 N1 102.9(4) 2 . ?
O1 Co3 N1 102.9(4) . . ?
O5 Co4 O5 95.3(7) 5_567 6_557 ?
O5 Co4 O5 95.3(7) 5_567 4_667 ?
O5 Co4 O5 95.3(6) 6_557 4_667 ?
O5 Co4 O4 92.7(6) 5_567 3_565 ?
O5 Co4 O4 79.3(6) 6_557 3_565 ?
O5 Co4 O4 170.7(6) 4_667 3_565 ?
O5 Co4 O4 79.3(6) 5_567 2_665 ?
O5 Co4 O4 170.7(6) 6_557 2_665 ?
O5 Co4 O4 92.7(6) 4_667 2_665 ?
O4 Co4 O4 93.3(7) 3_565 2_665 ?
O5 Co4 O4 170.7(6) 5_567 . ?
O5 Co4 O4 92.7(6) 6_557 . ?
O5 Co4 O4 79.3(6) 4_667 . ?
O4 Co4 O4 93.3(7) 3_565 . ?
O4 Co4 O4 93.3(7) 2_665 . ?
Co3 O1 Co1 119.7(5) . 5_556 ?
Co3 O1 Co1 120.3(5) . . ?
Co1 O1 Co1 93.7(4) 5_556 . ?
Co3 O1 H1 107.3 . . ?
Co1 O1 H1 107.3 5_556 . ?
Co1 O1 H1 107.3 . . ?
Co1 O2 Co1 99.5(5) 6_556 . ?
Co1 O2 Co2 96.9(4) 6_556 4_666 ?
Co1 O2 Co2 96.6(4) . 4_666 ?
Co1 O2 H2 119.6 6_556 . ?
Co1 O2 H2 119.6 . . ?
Co2 O2 H2 119.6 4_666 . ?
Co1 O3 Co2 97.1(4) 4_666 . ?
Co1 O3 Co1 95.4(4) 4_666 . ?
Co2 O3 Co1 95.8(4) . . ?
Co1 O3 H3 120.8 4_666 . ?
Co2 O3 H3 120.8 . . ?
Co1 O3 H3 120.8 . . ?
C2B N1 C2A 110.5(5) . . ?
C2B N1 Co3 122.1(3) . . ?
C2A N1 Co3 122.1(3) . . ?
C2B N1 H4 97.7 . . ?
C2A N1 H4 97.7 . . ?
Co3 N1 H4 97.7 . . ?
N1 C2A C2B 113.7(6) . 4_557 ?
N1 C2A H5 108.8 . . ?
C2B C2A H5 108.8 4_557 . ?
N1 C2A H6 108.8 . . ?
C2B C2A H6 108.8 4_557 . ?
H5 C2A H6 107.7 . . ?
N1 C2B C2A 113.7(6) . 4_557 ?
N1 C2B H7 108.8 . . ?
C2A C2B H7 108.8 4_557 . ?
N1 C2B H8 108.8 . . ?
C2A C2B H8 108.8 4_557 . ?
H7 C2B H8 107.7 . . ?
C1 O4 Co4 113.1(14) . . ?
C1 O5 Co4 111.2(14) . 4_667 ?
O5 C1 O4 123.5(14) . . ?
O5 C1 C1 120(3) . 4_667 ?
O4 C1 C1 116(3) . 4_667 ?
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 O2 2.055(11) 5_556 ?
Co1 O2 2.083(11) . ?
Co1 O3 2.085(10) 4_666 ?
Co1 O3 2.112(10) . ?
Co1 O1 2.149(11) 6_556 ?
Co1 O1 2.180(11) . ?
Co2 O3 2.100(10) 3_665 ?
Co2 O3 2.100(10) 2_655 ?
Co2 O3 2.100(10) . ?
Co2 O2 2.120(10) 6_656 ?
Co2 O2 2.120(11) 5_556 ?
Co2 O2 2.120(10) 4_666 ?
Co3 O1 1.957(11) 3 ?
Co3 O1 1.957(11) 2 ?
Co3 O1 1.957(11) . ?
Co3 N1 1.982(6) . ?
Co4 O5 2.129(17) 5_567 ?
Co4 O5 2.129(18) 6_557 ?
Co4 O5 2.129(18) 4_667 ?
Co4 O4 2.132(17) 3_565 ?
Co4 O4 2.132(18) 2_665 ?
Co4 O4 2.132(17) . ?
O1 Co1 2.149(11) 5_556 ?
O1 H1 0.9800 . ?
O2 Co1 2.055(11) 6_556 ?
O2 Co2 2.120(10) 4_666 ?
O2 H2 0.9800 . ?
O3 Co1 2.085(10) 4_666 ?
O3 H3 0.9800 . ?
N1 C2B 1.467(5) . ?
N1 C2A 1.467(5) . ?
N1 H4 0.9100 . ?
C2A C2B 1.519(5) 4_557 ?
C2A H5 0.9700 . ?
C2A H6 0.9700 . ?
C2B C2A 1.519(5) 4_557 ?
C2B H7 0.9700 . ?
C2B H8 0.9700 . ?
O4 C1 1.23(3) . ?
O5 C1 1.22(3) . ?
O5 Co4 2.129(17) 4_667 ?
C1 C1 1.563(19) 4_667 ?
