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#$Date: 2016-03-23 00:13:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179099 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/61/4306132.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_4306132
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         'C10 H12 Co Na2 O8'
_chemical_formula_sum            'C10 H12 Co Na2 O8'
_chemical_formula_weight         365.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 110.815(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5823(19)
_cell_length_b                   7.6716(10)
_cell_length_c                   10.4306(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.0
_cell_volume                     1315.1(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1906
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        no
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XSCANS (Siemens, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0268
_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)+(0.0267P)²+0.9602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                1318
_reflns_number_total             1512
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic801053p_si_002.cif
_cod_data_source_block           emp97
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4306132
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Co Co 0.0000 0.25650(5) 0.2500 0.02016(12) Uani 1 2 d S . .
Na1 Na 0.0000 0.5000 0.5000 0.0251(2) Uani 1 2 d S . .
Na2 Na 0.0000 -0.18084(15) 0.2500 0.0280(2) Uani 1 2 d S . .
O1 O 0.05821(8) 0.07807(19) 0.38577(13) 0.0275(3) Uani 1 1 d . . .
O2 O 0.05598(9) 0.22312(19) 0.56798(15) 0.0296(3) Uani 1 1 d . . .
O3 O 0.41200(9) -0.0754(2) 0.61837(15) 0.0356(4) Uani 1 1 d . . .
O4 O 0.41104(8) 0.11368(18) 0.77849(14) 0.0268(3) Uani 1 1 d . . .
C1 C 0.08172(10) 0.1040(2) 0.51520(18) 0.0197(3) Uani 1 1 d . . .
C2 C 0.14675(10) -0.0185(3) 0.60250(19) 0.0228(4) Uani 1 1 d . . .
H2A H 0.1335 -0.1371 0.5699 0.027 Uiso 1 1 calc R . .
H2B H 0.1492 -0.0133 0.6968 0.027 Uiso 1 1 calc R . .
C3 C 0.22943(10) 0.0327(3) 0.59557(19) 0.0240(4) Uani 1 1 d . . .
H3A H 0.2281 0.0172 0.5025 0.029 Uiso 1 1 calc R . .
H3B H 0.2397 0.1549 0.6191 0.029 Uiso 1 1 calc R . .
C4 C 0.29835(11) -0.0767(3) 0.6930(2) 0.0266(4) Uani 1 1 d . . .
H4A H 0.2965 -0.0710 0.7847 0.032 Uiso 1 1 calc R . .
H4B H 0.2915 -0.1975 0.6636 0.032 Uiso 1 1 calc R . .
C5 C 0.37969(10) -0.0106(3) 0.69504(19) 0.0221(4) Uani 1 1 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'
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'
Na Na 0.0362 0.0249 '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
O4 Co O4 119.06(8) 7_556 8_455 ?
O4 Co O1 118.74(6) 7_556 2 ?
O4 Co O1 102.85(6) 8_455 2 ?
O4 Co O1 102.85(6) 7_556 . ?
O4 Co O1 118.74(6) 8_455 . ?
O1 Co O1 92.20(8) 2 . ?
O4 Co Na1 93.31(4) 7_556 . ?
O4 Co Na1 49.58(4) 8_455 . ?
O1 Co Na1 146.85(4) 2 . ?
O1 Co Na1 88.30(4) . . ?
O4 Co Na1 49.58(4) 7_556 2 ?
O4 Co Na1 93.31(4) 8_455 2 ?
O1 Co Na1 88.30(4) 2 2 ?
O1 Co Na1 146.85(4) . 2 ?
Na1 Co Na1 108.768(14) . 2 ?
O4 Co Na2 120.47(4) 7_556 . ?
O4 Co Na2 120.47(4) 8_455 . ?
O1 Co Na2 46.10(4) 2 . ?
O1 Co Na2 46.10(4) . . ?
Na1 Co Na2 125.616(7) . . ?
Na1 Co Na2 125.616(7) 2 . ?
O2 Na1 O2 180.00(7) . 5_566 ?
O2 Na1 O3 95.57(6) . 7_556 ?
O2 Na1 O3 84.43(6) 5_566 7_556 ?
O2 Na1 O3 84.43(6) . 3_455 ?
O2 Na1 O3 95.57(6) 5_566 3_455 ?
O3 Na1 O3 180.00(4) 7_556 3_455 ?
O2 Na1 O4 88.77(5) . 4_556 ?
O2 Na1 O4 91.23(5) 5_566 4_556 ?
O3 Na1 O4 95.08(5) 7_556 4_556 ?
O3 Na1 O4 84.92(5) 3_455 4_556 ?
O2 Na1 O4 91.23(5) . 8_455 ?
O2 Na1 O4 88.77(5) 5_566 8_455 ?
O3 Na1 O4 84.92(5) 7_556 8_455 ?
O3 Na1 O4 95.08(5) 3_455 8_455 ?
O4 Na1 O4 180.0 4_556 8_455 ?
O2 Na1 Co 113.79(4) . 5_566 ?
O2 Na1 Co 66.21(4) 5_566 5_566 ?
O3 Na1 Co 118.06(4) 7_556 5_566 ?
O3 Na1 Co 61.94(4) 3_455 5_566 ?
O4 Na1 Co 37.70(3) 4_556 5_566 ?
O4 Na1 Co 142.30(3) 8_455 5_566 ?
O2 Na1 Co 66.21(4) . . ?
O2 Na1 Co 113.79(4) 5_566 . ?
O3 Na1 Co 61.94(4) 7_556 . ?
O3 Na1 Co 118.06(4) 3_455 . ?
O4 Na1 Co 142.30(3) 4_556 . ?
O4 Na1 Co 37.70(3) 8_455 . ?
Co Na1 Co 180.0 5_566 . ?
O2 Na1 Na2 137.10(4) . 1_565 ?
O2 Na1 Na2 42.90(4) 5_566 1_565 ?
O3 Na1 Na2 44.25(4) 7_556 1_565 ?
O3 Na1 Na2 135.75(4) 3_455 1_565 ?
O4 Na1 Na2 106.20(4) 4_556 1_565 ?
O4 Na1 Na2 73.80(4) 8_455 1_565 ?
Co Na1 Na2 101.187(17) 5_566 1_565 ?
Co Na1 Na2 78.813(17) . 1_565 ?
O2 Na1 Na2 42.90(4) . 5_556 ?
O2 Na1 Na2 137.10(4) 5_566 5_556 ?
O3 Na1 Na2 135.75(4) 7_556 5_556 ?
O3 Na1 Na2 44.25(4) 3_455 5_556 ?
O4 Na1 Na2 73.80(4) 4_556 5_556 ?
O4 Na1 Na2 106.20(4) 8_455 5_556 ?
Co Na1 Na2 78.813(17) 5_566 5_556 ?
Co Na1 Na2 101.187(18) . 5_556 ?
Na2 Na1 Na2 180.0 1_565 5_556 ?
O1 Na2 O1 71.21(7) . 2 ?
O1 Na2 O2 110.84(5) . 6 ?
O1 Na2 O2 81.92(5) 2 6 ?
O1 Na2 O2 81.92(5) . 5_556 ?
O1 Na2 O2 110.84(5) 2 5_556 ?
O2 Na2 O2 164.79(8) 6 5_556 ?
O1 Na2 O3 167.24(5) . 8_445 ?
O1 Na2 O3 103.86(5) 2 8_445 ?
O2 Na2 O3 79.42(5) 6 8_445 ?
O2 Na2 O3 89.19(5) 5_556 8_445 ?
O1 Na2 O3 103.86(5) . 7_546 ?
O1 Na2 O3 167.24(5) 2 7_546 ?
O2 Na2 O3 89.19(5) 6 7_546 ?
O2 Na2 O3 79.42(5) 5_556 7_546 ?
O3 Na2 O3 83.32(8) 8_445 7_546 ?
O1 Na2 C5 148.07(5) . 8_445 ?
O1 Na2 C5 113.40(5) 2 8_445 ?
O2 Na2 C5 101.06(5) 6 8_445 ?
O2 Na2 C5 66.76(5) 5_556 8_445 ?
O3 Na2 C5 22.61(5) 8_445 8_445 ?
O3 Na2 C5 77.19(6) 7_546 8_445 ?
O1 Na2 C5 113.40(5) . 7_546 ?
O1 Na2 C5 148.07(5) 2 7_546 ?
O2 Na2 C5 66.76(5) 6 7_546 ?
O2 Na2 C5 101.06(5) 5_556 7_546 ?
O3 Na2 C5 77.19(6) 8_445 7_546 ?
O3 Na2 C5 22.61(5) 7_546 7_546 ?
C5 Na2 C5 79.97(7) 8_445 7_546 ?
O1 Na2 Co 35.61(3) . . ?
O1 Na2 Co 35.61(3) 2 . ?
O2 Na2 Co 97.60(4) 6 . ?
O2 Na2 Co 97.60(4) 5_556 . ?
O3 Na2 Co 138.34(4) 8_445 . ?
O3 Na2 Co 138.34(4) 7_546 . ?
C5 Na2 Co 140.01(4) 8_445 . ?
C5 Na2 Co 140.01(4) 7_546 . ?
O1 Na2 Na1 150.53(4) . 2_545 ?
O1 Na2 Na1 104.03(3) 2 2_545 ?
O2 Na2 Na1 40.59(3) 6 2_545 ?
O2 Na2 Na1 125.32(5) 5_556 2_545 ?
O3 Na2 Na1 41.31(4) 8_445 2_545 ?
O3 Na2 Na1 74.24(4) 7_546 2_545 ?
C5 Na2 Na1 61.16(4) 8_445 2_545 ?
C5 Na2 Na1 55.49(4) 7_546 2_545 ?
Co Na2 Na1 133.197(14) . 2_545 ?
O1 Na2 Na1 104.03(3) . 1_545 ?
O1 Na2 Na1 150.53(4) 2 1_545 ?
O2 Na2 Na1 125.32(5) 6 1_545 ?
O2 Na2 Na1 40.59(3) 5_556 1_545 ?
O3 Na2 Na1 74.24(4) 8_445 1_545 ?
O3 Na2 Na1 41.31(4) 7_546 1_545 ?
C5 Na2 Na1 55.49(4) 8_445 1_545 ?
C5 Na2 Na1 61.16(4) 7_546 1_545 ?
Co Na2 Na1 133.197(14) . 1_545 ?
Na1 Na2 Na1 93.61(3) 2_545 1_545 ?
C1 O1 Co 122.67(13) . . ?
C1 O1 Na2 130.55(12) . . ?
Co O1 Na2 98.30(5) . . ?
C1 O2 Na1 135.91(12) . . ?
C1 O2 Na2 124.07(12) . 5_556 ?
Na1 O2 Na2 96.50(5) . 5_556 ?
C5 O3 Na1 140.68(15) . 3_545 ?
C5 O3 Na2 106.36(12) . 7_546 ?
Na1 O3 Na2 94.44(5) 3_545 7_546 ?
C5 O4 Co 116.73(12) . 7_556 ?
C5 O4 Na1 110.75(11) . 4_546 ?
Co O4 Na1 92.72(5) 7_556 4_546 ?
O2 C1 O1 123.67(17) . . ?
O2 C1 C2 120.77(16) . . ?
O1 C1 C2 115.52(16) . . ?
C1 C2 C3 109.87(15) . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C2 111.72(15) . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C5 C4 C3 110.42(16) . . ?
C5 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
C5 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
O3 C5 O4 123.66(17) . . ?
O3 C5 C4 120.39(18) . . ?
O4 C5 C4 115.96(16) . . ?
O3 C5 Na2 51.03(10) . 7_546 ?
O4 C5 Na2 110.15(11) . 7_546 ?
C4 C5 Na2 109.14(12) . 7_546 ?
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
Co O4 1.9639(14) 7_556 ?
Co O4 1.9639(14) 8_455 ?
Co O1 1.9740(13) 2 ?
Co O1 1.9740(13) . ?
Co Na1 3.2077(3) . ?
Co Na1 3.2077(4) 2 ?
Co Na2 3.3551(13) . ?
Na1 O2 2.3425(14) . ?
Na1 O2 2.3425(14) 5_566 ?
Na1 O3 2.3686(15) 7_556 ?
Na1 O3 2.3686(15) 3_455 ?
Na1 O4 2.4448(14) 4_556 ?
Na1 O4 2.4448(14) 8_455 ?
Na1 Co 3.2077(4) 5_566 ?
Na1 Na2 3.5770(9) 1_565 ?
Na1 Na2 3.5770(9) 5_556 ?
Na2 O1 2.4430(17) . ?
Na2 O1 2.4430(17) 2 ?
Na2 O2 2.4508(15) 6 ?
Na2 O2 2.4508(15) 5_556 ?
Na2 O3 2.5035(19) 8_445 ?
Na2 O3 2.5035(19) 7_546 ?
Na2 C5 3.090(2) 8_445 ?
Na2 C5 3.090(2) 7_546 ?
Na2 Na1 3.5770(8) 2_545 ?
Na2 Na1 3.5770(8) 1_545 ?
O1 C1 1.279(2) . ?
O2 C1 1.233(2) . ?
O2 Na2 2.4508(15) 5_556 ?
O3 C5 1.238(2) . ?
O3 Na1 2.3686(15) 3_545 ?
O3 Na2 2.5035(19) 7_546 ?
O4 C5 1.276(2) . ?
O4 Co 1.9639(14) 7_556 ?
O4 Na1 2.4448(14) 4_546 ?
C1 C2 1.510(2) . ?
C2 C3 1.532(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.526(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.510(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 Na2 3.090(2) 7_546 ?
