#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:09:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180005 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/99/7029974.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_7029974
loop_
_publ_author_name
'Li, Zhong-Yi'
'Yang, Jing-Si'
'Liu, Rui-Bin'
'Zhang, Jian-Jun'
'Liu, Shu-Qin'
'Ni, Jun'
'Duan, Chun-Ying'
_publ_section_title
;
 Two one-dimensional compounds based on pyramidal {TbCu4} units and
 formate ligand: chair-like [(H2O)2(ClO4)2]2- clusters and slow relaxation
 of magnetization.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13264
_journal_page_last               13266
_journal_paper_doi               10.1039/c2dt32147e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C5 H29 Cl2 Cu4 O32 Tb'
_chemical_formula_weight         1085.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 113.266(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4356(19)
_cell_length_b                   18.837(4)
_cell_length_c                   10.116(2)
_cell_measurement_reflns_used    3798
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.225
_cell_measurement_theta_min      2.192
_cell_volume                     1476.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7209
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    5.497
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2000
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.441
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2673
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0358P)²+4.1455P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                2434
_reflns_number_total             2673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32147e.txt
_cod_data_source_block           1_L
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1476.7(6)
_cod_original_sg_symbol_H-M      'P2(1)/m '
_cod_database_code               7029974
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Tb1 Tb 0.87494(4) 0.7500 0.52684(4) 0.01866(13) Uani 1 2 d S
Cu1 Cu 0.44788(11) 0.7500 0.26657(10) 0.0227(2) Uani 1 2 d S
Cu2 Cu 0.54019(8) 0.63366(4) 0.50408(7) 0.02323(18) Uani 1 1 d .
Cu3 Cu 0.62932(12) 0.7500 0.73637(10) 0.0234(2) Uani 1 2 d S
Cl1 Cl 0.7811(2) 0.55266(9) 0.15489(19) 0.0453(4) Uani 1 1 d .
O1 O 0.3452(5) 0.5912(2) 0.3439(4) 0.0347(10) Uani 1 1 d .
O2 O 0.2757(5) 0.6761(2) 0.1742(4) 0.0376(10) Uani 1 1 d .
O3 O 0.5257(5) 0.6770(2) 0.8158(4) 0.0359(10) Uani 1 1 d .
O4 O 0.4461(6) 0.5951(2) 0.6408(4) 0.0370(10) Uani 1 1 d .
O5 O 1.3997(6) 0.7500 0.4962(6) 0.0278(12) Uani 1 2 d S
O6 O 1.1699(7) 0.7500 0.5509(7) 0.0418(16) Uani 1 2 d S
O7 O 0.6259(5) 0.68030(19) 0.3715(4) 0.0215(8) Uani 1 1 d D
H7A H 0.638(7) 0.652(3) 0.312(5) 0.026 Uiso 1 1 d D
O8 O 0.7350(4) 0.68077(19) 0.6534(4) 0.0205(7) Uani 1 1 d D
H8A H 0.788(7) 0.651(2) 0.715(5) 0.025 Uiso 1 1 d D
O9 O 0.5421(10) 0.7500 0.0700(7) 0.0463(17) Uani 1 2 d SD
O10 O 0.7134(6) 0.5321(2) 0.5161(5) 0.0348(9) Uani 1 1 d D
H10A H 0.732(8) 0.511(3) 0.594(3) 0.042 Uiso 1 1 d D
H10B H 0.659(8) 0.505(3) 0.446(4) 0.042 Uiso 1 1 d D
O11 O 0.9251(12) 0.7500 0.9679(8) 0.0559(19) Uani 1 2 d SD
H11A H 0.935(11) 0.712(3) 1.015(8) 0.067 Uiso 1 1 d D
O12 O 0.8757(8) 0.7500 0.2863(7) 0.0472(18) Uani 1 2 d SD
H12A H 0.770(4) 0.7500 0.227(7) 0.057 Uiso 1 2 d SD
H12B H 0.936(9) 0.7500 0.235(8) 0.057 Uiso 1 2 d SD
O13 O 0.9741(5) 0.6279(2) 0.5322(6) 0.0409(11) Uani 1 1 d D
H13A H 1.069(5) 0.611(3) 0.536(8) 0.049 Uiso 1 1 d D
H13B H 0.909(6) 0.593(2) 0.530(8) 0.049 Uiso 1 1 d D
O14 O 1.0799(8) 0.7500 0.7736(7) 0.0509(19) Uani 1 2 d SD
H14A H 1.053(10) 0.7500 0.846(6) 0.061 Uiso 1 2 d SD
H14B H 1.189(3) 0.7500 0.803(9) 0.061 Uiso 1 2 d SD
O15 O 1.0840(10) 0.4154(5) 0.1480(8) 0.093(2) Uani 1 1 d D
H15A H 0.992(8) 0.431(5) 0.151(11) 0.111 Uiso 1 1 d D
H15B H 1.109(12) 0.437(5) 0.086(9) 0.111 Uiso 1 1 d D
O16 O 0.6275(8) 0.5756(4) 0.1651(9) 0.098(3) Uani 1 1 d .
O17 O 0.7479(11) 0.5145(5) 0.0271(9) 0.113(3) Uani 1 1 d .
O18 O 0.8839(12) 0.6116(4) 0.1590(11) 0.120(3) Uani 1 1 d .
O19 O 0.8687(14) 0.5091(5) 0.2707(10) 0.138(4) Uani 1 1 d .
C1 C 0.2679(8) 0.6157(4) 0.2201(7) 0.0363(15) Uani 1 1 d .
H1A H 0.183(9) 0.589(4) 0.164(7) 0.044 Uiso 1 1 d .
C2 C 0.4598(8) 0.6198(3) 0.7599(7) 0.0373(15) Uani 1 1 d .
H2A H 0.4152 0.5919 0.8129 0.045 Uiso 1 1 calc R
C3 C 1.2423(11) 0.7500 0.4741(11) 0.062(4) Uani 1 2 d S
H3A H 1.1692 0.7500 0.3771 0.074 Uiso 1 2 calc SR
H9A H 0.516(13) 0.7135(5) 0.017(4) 0.11(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'
O O 0.0106 0.0060 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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
O6 Tb1 O14 66.7(2) . .
O6 Tb1 O8 130.13(14) . 4_575
O14 Tb1 O8 75.75(15) . 4_575
O6 Tb1 O8 130.13(13) . .
O14 Tb1 O8 75.75(15) . .
O8 Tb1 O8 64.79(17) 4_575 .
O6 Tb1 O12 72.0(2) . .
O14 Tb1 O12 138.6(2) . .
O8 Tb1 O12 135.92(12) 4_575 .
O8 Tb1 O12 135.92(12) . .
O6 Tb1 O13 70.47(10) . .
O14 Tb1 O13 82.97(13) . .
O8 Tb1 O13 136.58(14) 4_575 .
O8 Tb1 O13 73.53(13) . .
O12 Tb1 O13 83.46(13) . .
O6 Tb1 O13 70.47(10) . 4_575
O14 Tb1 O13 82.97(13) . 4_575
O8 Tb1 O13 73.53(13) 4_575 4_575
O8 Tb1 O13 136.58(14) . 4_575
O12 Tb1 O13 83.46(13) . 4_575
O13 Tb1 O13 140.9(2) . 4_575
O6 Tb1 O7 131.04(13) . .
O14 Tb1 O7 138.34(12) . .
O8 Tb1 O7 98.83(12) 4_575 .
O8 Tb1 O7 65.11(12) . .
O12 Tb1 O7 72.48(14) . .
O13 Tb1 O7 73.06(14) . .
O13 Tb1 O7 135.97(14) 4_575 .
O6 Tb1 O7 131.04(13) . 4_575
O14 Tb1 O7 138.34(12) . 4_575
O8 Tb1 O7 65.11(12) 4_575 4_575
O8 Tb1 O7 98.83(12) . 4_575
O12 Tb1 O7 72.48(14) . 4_575
O13 Tb1 O7 135.97(15) . 4_575
O13 Tb1 O7 73.06(14) 4_575 4_575
O7 Tb1 O7 64.83(17) . 4_575
O6 Tb1 Cu3 140.85(15) . .
O14 Tb1 Cu3 74.16(15) . .
O8 Tb1 Cu3 32.41(8) 4_575 .
O8 Tb1 Cu3 32.41(8) . .
O12 Tb1 Cu3 147.19(14) . .
O13 Tb1 Cu3 105.44(11) . .
O13 Tb1 Cu3 105.44(11) 4_575 .
O7 Tb1 Cu3 79.96(8) . .
O7 Tb1 Cu3 79.96(8) 4_575 .
O6 Tb1 Cu2 141.347(15) . .
O14 Tb1 Cu2 107.30(11) . .
O8 Tb1 Cu2 79.89(8) 4_575 .
O8 Tb1 Cu2 32.36(8) . .
O12 Tb1 Cu2 104.71(11) . .
O13 Tb1 Cu2 70.90(10) . .
O13 Tb1 Cu2 148.18(10) 4_575 .
O7 Tb1 Cu2 32.77(8) . .
O7 Tb1 Cu2 80.13(9) 4_575 .
Cu3 Tb1 Cu2 52.149(17) . .
O6 Tb1 Cu2 141.347(15) . 4_575
O14 Tb1 Cu2 107.30(11) . 4_575
O8 Tb1 Cu2 32.36(8) 4_575 4_575
O8 Tb1 Cu2 79.89(8) . 4_575
O12 Tb1 Cu2 104.71(11) . 4_575
O13 Tb1 Cu2 148.18(10) . 4_575
O13 Tb1 Cu2 70.90(10) 4_575 4_575
O7 Tb1 Cu2 80.13(8) . 4_575
O7 Tb1 Cu2 32.77(8) 4_575 4_575
Cu3 Tb1 Cu2 52.149(17) . 4_575
Cu2 Tb1 Cu2 77.29(3) . 4_575
O7 Cu1 O7 84.1(2) 4_575 .
O7 Cu1 O2 175.87(17) 4_575 .
O7 Cu1 O2 92.69(17) . .
O7 Cu1 O2 92.69(17) 4_575 4_575
O7 Cu1 O2 175.87(17) . 4_575
O2 Cu1 O2 90.4(3) . 4_575
O7 Cu1 O9 90.85(17) 4_575 .
O7 Cu1 O9 90.85(17) . .
O2 Cu1 O9 91.75(19) . .
O2 Cu1 O9 91.75(19) 4_575 .
O7 Cu1 Tb1 42.05(11) 4_575 .
O7 Cu1 Tb1 42.05(11) . .
O2 Cu1 Tb1 134.57(13) . .
O2 Cu1 Tb1 134.57(13) 4_575 .
O9 Cu1 Tb1 92.49(19) . .
O8 Cu2 O7 84.29(15) . .
O8 Cu2 O1 175.93(16) . .
O7 Cu2 O1 91.90(16) . .
O8 Cu2 O4 94.22(16) . .
O7 Cu2 O4 174.79(17) . .
O1 Cu2 O4 89.46(17) . .
O8 Cu2 O10 90.78(15) . .
O7 Cu2 O10 90.60(15) . .
O1 Cu2 O10 90.67(17) . .
O4 Cu2 O10 94.41(17) . .
O8 Cu2 Tb1 41.87(10) . .
O7 Cu2 Tb1 42.44(11) . .
O1 Cu2 Tb1 134.26(12) . .
O4 Cu2 Tb1 135.71(12) . .
O10 Cu2 Tb1 92.11(11) . .
O8 Cu3 O8 84.1(2) . 4_575
O8 Cu3 O3 177.55(16) . 4_575
O8 Cu3 O3 93.49(16) 4_575 4_575
O8 Cu3 O3 93.49(17) . .
O8 Cu3 O3 177.55(16) 4_575 .
O3 Cu3 O3 88.9(3) 4_575 .
O8 Cu3 O5 83.63(14) . 1_455
O8 Cu3 O5 83.63(14) 4_575 1_455
O3 Cu3 O5 95.80(16) 4_575 1_455
O3 Cu3 O5 95.80(16) . 1_455
O8 Cu3 Tb1 42.06(11) . .
O8 Cu3 Tb1 42.06(11) 4_575 .
O3 Cu3 Tb1 135.49(13) 4_575 .
O3 Cu3 Tb1 135.49(13) . .
O5 Cu3 Tb1 79.84(12) 1_455 .
O19 Cl1 O18 109.1(7) . .
O19 Cl1 O17 108.7(6) . .
O18 Cl1 O17 109.2(5) . .
O19 Cl1 O16 108.7(6) . .
O18 Cl1 O16 109.4(5) . .
O17 Cl1 O16 111.7(5) . .
C1 O1 Cu2 127.6(4) . .
C1 O2 Cu1 127.7(4) . .
C2 O3 Cu3 127.8(4) . .
C2 O4 Cu2 128.6(4) . .
C3 O5 Cu3 123.0(6) . 1_655
C3 O6 Tb1 136.8(6) . .
Cu1 O7 Cu2 105.03(16) . .
Cu1 O7 Tb1 105.53(15) . .
Cu2 O7 Tb1 104.79(15) . .
Cu1 O7 H7A 108(4) . .
Cu2 O7 H7A 113(4) . .
Tb1 O7 H7A 119(4) . .
Cu3 O8 Cu2 104.42(16) . .
Cu3 O8 Tb1 105.53(15) . .
Cu2 O8 Tb1 105.77(15) . .
Cu3 O8 H8A 110(4) . .
Cu2 O8 H8A 108(4) . .
Tb1 O8 H8A 122(4) . .
Cu1 O9 H9A 116(6) . .
Cu2 O10 H10A 109(4) . .
Cu2 O10 H10B 109(5) . .
H10A O10 H10B 110(3) . .
Tb1 O12 H12A 107(6) . .
Tb1 O12 H12B 147(6) . .
H12A O12 H12B 106(3) . .
Tb1 O13 H13A 132(4) . .
Tb1 O13 H13B 121(4) . .
H13A O13 H13B 107(3) . .
Tb1 O14 H14A 125(6) . .
Tb1 O14 H14B 127(6) . .
H14A O14 H14B 108(3) . .
H15A O15 H15B 111(4) . .
O2 C1 O1 129.1(6) . .
O2 C1 H1A 115(5) . .
O1 C1 H1A 114(5) . .
O3 C2 O4 127.9(5) . .
O3 C2 H2A 116.1 . .
O4 C2 H2A 116.0 . .
O6 C3 O5 132.7(10) . .
O6 C3 H3A 113.6 . .
O5 C3 H3A 113.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O6 2.402(5) .
Tb1 O14 2.411(6) .
Tb1 O8 2.434(4) 4_575
Tb1 O8 2.434(4) .
Tb1 O12 2.436(6) .
Tb1 O13 2.440(4) .
Tb1 O13 2.440(4) 4_575
Tb1 O7 2.449(4) .
Tb1 O7 2.449(4) 4_575
Tb1 Cu3 3.5007(10) .
Tb1 Cu2 3.5094(9) .
Tb1 Cu2 3.5094(9) 4_575
Cu1 O7 1.961(4) 4_575
Cu1 O7 1.961(4) .
Cu1 O2 1.962(4) .
Cu1 O2 1.962(4) 4_575
Cu1 O9 2.415(6) .
Cu2 O8 1.952(4) .
Cu2 O7 1.965(4) .
Cu2 O1 1.967(4) .
Cu2 O4 1.984(4) .
Cu2 O10 2.381(4) .
Cu3 O8 1.947(4) .
Cu3 O8 1.947(4) 4_575
Cu3 O3 1.964(4) 4_575
Cu3 O3 1.964(4) .
Cu3 O5 2.437(6) 1_455
Cl1 O19 1.381(7) .
Cl1 O18 1.400(7) .
Cl1 O17 1.407(6) .
Cl1 O16 1.408(6) .
O1 C1 1.250(8) .
O2 C1 1.240(8) .
O3 C2 1.241(7) .
O4 C2 1.254(7) .
O5 C3 1.257(10) .
O5 Cu3 2.437(5) 1_655
O6 C3 1.163(11) .
O7 H7A 0.84(2) .
O8 H8A 0.84(2) .
O9 H9A 0.84(2) .
O10 H10A 0.84(2) .
O10 H10B 0.84(2) .
O11 H11A 0.84(2) .
O12 H12A 0.85(2) .
O12 H12B 0.86(2) .
O13 H13A 0.85(2) .
O13 H13B 0.86(2) .
O14 H14A 0.85(2) .
O14 H14B 0.85(2) .
O15 H15A 0.85(2) .
O15 H15B 0.84(2) .
C1 H1A 0.87(7) .
C2 H2A 0.9300 .
C3 H3A 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O16 0.84(2) 2.05(2) 2.876(7) 170(6) .
O8 H8A O15 0.84(2) 1.85(2) 2.688(7) 177(6) 3_766
O10 H10A O1 0.84(2) 2.20(4) 2.862(6) 136(5) 3_666
O10 H10B O4 0.84(2) 2.13(4) 2.896(6) 152(5) 3_666
O11 H11A O18 0.84(2) 2.53(3) 3.344(10) 164(8) 1_556
O12 H12A O9 0.85(2) 1.96(3) 2.800(10) 172(8) .
O13 H13B O10 0.86(2) 1.97(2) 2.800(6) 165(6) .
O14 H14A O11 0.85(2) 1.94(3) 2.756(10) 163(8) .
O15 H15A O19 0.85(2) 2.38(7) 3.120(11) 146(10) .
O15 H15A O17 0.85(2) 2.49(6) 3.206(11) 143(8) .
O15 H15B O17 0.84(2) 2.17(3) 2.980(11) 162(9) 3_765
O9 H9A O3 0.84(2) 2.18(6) 2.872(7) 139(6) 1_554
