#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:13:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179099 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/61/4306134.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_4306134
loop_
_publ_author_name
'Yue-Qing Zheng'
'Jian-Li Lin'
'Wei Xu'
'Hong-Zhen Xie'
'Jie Sun'
'Xian-Wen Wang'
_publ_contact_author_address
;
      State Key Lab. Base of Novel Functional Mater. & Prep. Science
      Faculty of Materials Science and Chemical Engineering
      Ningbo University
      Ningbo 315211
      P. R. China

;
_publ_contact_author_email       zhengyueqing@nbu.edu.cn
_publ_contact_author_fax         '86 574 87600747'
_publ_contact_author_name        'Yue-Qing Zheng'
_publ_contact_author_phone       '86 574 87600747'
_publ_section_title
;
A Family of New Glutarate Compounds: Synthesis, Crystal Structures of:
Co(H2O)5L(1), Na2[CoL2] (2), Na2[L(H2L)4/2] (3), {[Co3(H2O)6L2](HL)2}.4H2O
(4), {[Co3(H2O)6L2](HL)2}.10H2O (5), {[Co3(H2O)6L2]L2/2}.4H2O (6), and
Na2{[Co3(H2O)2]L8/2].6H2O (7), and Magnetic Properties of 1 and 2 with H2L
= HOOC-(CH2)3-COOH
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10280
_journal_page_last               10287
_journal_paper_doi               10.1021/ic801053p
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C20 H38 Co3 O22, 4(H2 O)'
_chemical_formula_sum            'C20 H46 Co3 O26'
_chemical_formula_weight         879.36
_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           SHELXL-97
_cell_angle_alpha                95.07(3)
_cell_angle_beta                 107.35(3)
_cell_angle_gamma                113.69(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3617(17)
_cell_length_b                   9.4550(19)
_cell_length_c                   12.628(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.0
_cell_volume                     847.5(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'θ/2θ scans'
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7948
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.550
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XSCANS (Siemens, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             455
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.683
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0796P)²+0.3335P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                3265
_reflns_number_total             3825
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic801053p_si_004.cif
_cod_data_source_block           shx97
_cod_database_code               4306134
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.0000 0.5000 0.01977(17) Uani 1 2 d S . .
Co2 Co 0.39209(6) 0.10540(4) 0.25971(3) 0.02400(16) Uani 1 1 d . . .
O1 O 0.9525(4) 0.2536(3) 0.81915(19) 0.0398(6) Uani 1 1 d . . .
O2 O 0.7267(3) 0.0834(2) 0.66216(17) 0.0252(4) Uani 1 1 d . . .
C1 C 0.8734(4) 0.2152(3) 0.7140(2) 0.0247(6) Uani 1 1 d . . .
C2 C 0.9512(4) 0.3292(4) 0.6453(3) 0.0299(7) Uani 1 1 d . . .
H2A H 0.8974 0.2743 0.5653 0.036 Uiso 1 1 calc R . .
H2B H 1.0862 0.3680 0.6710 0.036 Uiso 1 1 calc R . .
C3 C 0.9056(5) 0.4700(3) 0.6591(3) 0.0335(7) Uani 1 1 d . . .
H3A H 0.9531 0.5205 0.7396 0.040 Uiso 1 1 calc R . .
H3B H 0.9686 0.5477 0.6216 0.040 Uiso 1 1 calc R . .
C4 C 0.6971(5) 0.4186(3) 0.6088(2) 0.0276(6) Uani 1 1 d . . .
H4A H 0.6721 0.5074 0.6277 0.033 Uiso 1 1 calc R . .
H4B H 0.6320 0.3340 0.6411 0.033 Uiso 1 1 calc R . .
C5 C 0.6260(4) 0.3607(3) 0.4804(2) 0.0231(6) Uani 1 1 d . . .
O3 O 0.6594(4) 0.4614(2) 0.42276(19) 0.0377(6) Uani 1 1 d . . .
O4 O 0.5395(3) 0.2115(2) 0.43640(16) 0.0237(4) Uani 1 1 d . . .
O5 O 0.2174(4) -0.0153(3) 0.09118(19) 0.0413(6) Uani 1 1 d . . .
H5A H 0.1508 -0.0951 0.1079 0.050 Uiso 1 1 d R . .
H5B H 0.2441 -0.0323 0.0387 0.050 Uiso 1 1 d R . .
O6 O 0.5369(3) 0.3043(3) 0.2057(2) 0.0352(5) Uani 1 1 d . . .
H6A H 0.4701 0.3402 0.1643 0.042 Uiso 1 1 d R . .
H6B H 0.5848 0.3733 0.2601 0.042 Uiso 1 1 d R . .
O7 O 0.1901(3) 0.1796(3) 0.2608(2) 0.0380(6) Uani 1 1 d . . .
H7A H 0.1137 0.1731 0.2119 0.046 Uiso 1 1 d R . .
H7B H 0.1596 0.1788 0.3137 0.046 Uiso 1 1 d R . .
O8 O 0.6540(3) -0.0511(2) 0.41660(17) 0.0260(4) Uani 1 1 d . . .
O9 O 0.5970(3) 0.0387(3) 0.25825(18) 0.0311(5) Uani 1 1 d . . .
C6 C 0.6658(4) -0.0355(3) 0.3204(2) 0.0227(6) Uani 1 1 d . . .
C7 C 0.7596(4) -0.1186(3) 0.2736(3) 0.0257(6) Uani 1 1 d . . .
H7C H 0.8601 -0.1197 0.3360 0.031 Uiso 1 1 calc R . .
H7D H 0.8139 -0.0611 0.2233 0.031 Uiso 1 1 calc R . .
C8 C 0.6174(4) -0.2902(4) 0.2075(3) 0.0283(6) Uani 1 1 d . . .
H8A H 0.6811 -0.3412 0.1786 0.034 Uiso 1 1 calc R . .
H8B H 0.5687 -0.3485 0.2593 0.034 Uiso 1 1 calc R . .
C9 C 0.4554(5) -0.2983(4) 0.1085(3) 0.0381(8) Uani 1 1 d . . .
H9A H 0.3883 -0.2521 0.1382 0.046 Uiso 1 1 calc R . .
H9B H 0.5053 -0.2343 0.0595 0.046 Uiso 1 1 calc R . .
C10 C 0.3195(5) -0.4634(4) 0.0380(3) 0.0342(7) Uani 1 1 d . . .
O10 O 0.3230(5) -0.5840(3) 0.0581(3) 0.0646(10) Uani 1 1 d . . .
O11 O 0.1901(4) -0.4637(3) -0.0522(2) 0.0406(6) Uani 1 1 d . . .
H H 0.111(6) -0.550(5) -0.086(4) 0.049 Uiso 1 1 d . . .
O12 O 0.2072(5) -0.1618(3) -0.1127(2) 0.0549(8) Uani 1 1 d . . .
H12A H 0.1946 -0.2430 -0.0978 0.066 Uiso 1 1 d R . .
H12B H 0.2622 -0.1402 -0.1521 0.066 Uiso 1 1 d R . .
O13 O 0.1523(4) 0.2122(3) 0.4609(2) 0.0395(6) Uani 1 1 d . . .
H13A H 0.1995 0.1679 0.4958 0.047 Uiso 1 1 d R . .
H13B H 0.2131 0.3039 0.4983 0.047 Uiso 1 1 d 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'
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
O8 Co1 O8 180.000(1) . 2_656 ?
O8 Co1 O2 87.83(9) . 2_656 ?
O8 Co1 O2 92.17(9) 2_656 2_656 ?
O8 Co1 O2 92.17(9) . . ?
O8 Co1 O2 87.83(9) 2_656 . ?
O2 Co1 O2 180.0 2_656 . ?
O8 Co1 O4 91.33(8) . . ?
O8 Co1 O4 88.67(8) 2_656 . ?
O2 Co1 O4 75.98(8) 2_656 . ?
O2 Co1 O4 104.02(9) . . ?
O8 Co1 O4 88.67(8) . 2_656 ?
O8 Co1 O4 91.32(8) 2_656 2_656 ?
O2 Co1 O4 104.02(9) 2_656 2_656 ?
O2 Co1 O4 75.98(8) . 2_656 ?
O4 Co1 O4 180.00(5) . 2_656 ?
O9 Co2 O7 178.25(9) . . ?
O9 Co2 O5 94.94(10) . . ?
O7 Co2 O5 85.46(10) . . ?
O9 Co2 O6 86.88(9) . . ?
O7 Co2 O6 91.42(10) . . ?
O5 Co2 O6 90.64(10) . . ?
O9 Co2 O4 89.31(9) . . ?
O7 Co2 O4 90.47(9) . . ?
O5 Co2 O4 172.68(9) . . ?
O6 Co2 O4 95.55(9) . . ?
O9 Co2 O2 90.96(9) . 2_656 ?
O7 Co2 O2 90.68(9) . 2_656 ?
O5 Co2 O2 97.07(9) . 2_656 ?
O6 Co2 O2 172.15(9) . 2_656 ?
O4 Co2 O2 76.86(8) . 2_656 ?
C1 O2 Co1 134.45(18) . . ?
C1 O2 Co2 125.40(18) . 2_656 ?
Co1 O2 Co2 98.82(9) . 2_656 ?
O1 C1 O2 122.2(3) . . ?
O1 C1 C2 118.7(3) . . ?
O2 C1 C2 119.2(3) . . ?
C1 C2 C3 110.4(3) . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C2 111.9(3) . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 C5 109.8(3) . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O3 C5 O4 122.9(3) . . ?
O3 C5 C4 118.2(3) . . ?
O4 C5 C4 118.9(2) . . ?
C5 O4 Co2 124.96(18) . . ?
C5 O4 Co1 135.56(18) . . ?
Co2 O4 Co1 99.45(8) . . ?
Co2 O5 H5A 94.8 . . ?
Co2 O5 H5B 129.2 . . ?
H5A O5 H5B 115.3 . . ?
Co2 O6 H6A 115.6 . . ?
Co2 O6 H6B 103.6 . . ?
H6A O6 H6B 97.3 . . ?
Co2 O7 H7A 126.8 . . ?
Co2 O7 H7B 119.3 . . ?
H7A O7 H7B 108.0 . . ?
C6 O8 Co1 131.96(19) . . ?
C6 O9 Co2 130.62(19) . . ?
O9 C6 O8 124.7(3) . . ?
O9 C6 C7 117.5(2) . . ?
O8 C6 C7 117.7(2) . . ?
C6 C7 C8 110.6(2) . . ?
C6 C7 H7C 109.5 . . ?
C8 C7 H7C 109.5 . . ?
C6 C7 H7D 109.5 . . ?
C8 C7 H7D 109.5 . . ?
H7C C7 H7D 108.1 . . ?
C9 C8 C7 112.6(3) . . ?
C9 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 114.1(3) . . ?
C10 C9 H9A 108.7 . . ?
C8 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
C8 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
O10 C10 O11 122.0(3) . . ?
O10 C10 C9 126.0(3) . . ?
O11 C10 C9 112.0(3) . . ?
C10 O11 H 113(3) . . ?
H12A O12 H12B 112.5 . . ?
H13A O13 H13B 103.4 . . ?
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 O8 2.054(2) . ?
Co1 O8 2.054(2) 2_656 ?
Co1 O2 2.146(2) 2_656 ?
Co1 O2 2.146(2) . ?
Co1 O4 2.1596(19) . ?
Co1 O4 2.1596(19) 2_656 ?
Co2 O9 2.054(2) . ?
Co2 O7 2.076(2) . ?
Co2 O5 2.084(3) . ?
Co2 O6 2.087(2) . ?
Co2 O4 2.115(2) . ?
Co2 O2 2.149(2) 2_656 ?
O1 C1 1.237(4) . ?
O2 C1 1.278(4) . ?
O2 Co2 2.149(2) 2_656 ?
C1 C2 1.509(4) . ?
C2 C3 1.534(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.512(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.513(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O3 1.243(3) . ?
C5 O4 1.274(3) . ?
O5 H5A 0.8278 . ?
O5 H5B 0.7830 . ?
O6 H6A 0.8431 . ?
O6 H6B 0.7780 . ?
O7 H7A 0.7202 . ?
O7 H7B 0.7830 . ?
O8 C6 1.265(3) . ?
O9 C6 1.261(3) . ?
C6 C7 1.507(4) . ?
C7 C8 1.536(4) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C8 C9 1.514(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.499(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 O10 1.200(4) . ?
C10 O11 1.315(4) . ?
O11 H 0.79(4) . ?
O12 H12A 0.7800 . ?
O12 H12B 0.7619 . ?
O13 H13A 0.7660 . ?
O13 H13B 0.8142 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -65.3(3) . . . . ?
C2 C3 C4 C5 -66.8(3) . . . . ?
C6 C7 C8 C9 59.0(3) . . . . ?
C7 C8 C9 C10 176.8(3) . . . . ?
