#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/43/2224331.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_2224331
loop_
_publ_author_name
'Wei, Dan-Yi'
'Zhang, Yan-Guang'
'Wang, Mei-Li'
'Zhu, Zhen-Ke'
_publ_section_title
catena-Poly[diaquatris(μ₃-biphenyl-2,2-dicarboxylato)disamarium(III)]
_journal_coeditor_code           JH2091
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1553
_journal_page_last               m1554
_journal_paper_doi               10.1107/S1600536809046625
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Sm2 (C14 H8 O4)3 (H2 O)2]'
_chemical_formula_moiety         'C42 H28 O14 Sm2'
_chemical_formula_sum            'C42 H28 O14 Sm2'
_chemical_formula_weight         1057.34
_chemical_name_systematic
catena-Poly[diaquatris(μ₃-biphenyl-2,2-dicarboxylato)disamarium(III)]
_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                 103.94(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.776(4)
_cell_length_b                   21.441(4)
_cell_length_c                   8.2660(17)
_cell_measurement_reflns_used    12337
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      3.03
_cell_volume                     3573.7(13)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15001
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.330
_exptl_absorpt_correction_T_max  0.409
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.311
_refine_diff_density_min         -1.910
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+89.0505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                3238
_reflns_number_total             3962
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            jh2091.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2224331
_cod_database_fobs_code          2224331
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_type_symbol
_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
Sm Sm1 0.0000 0.20641(2) 0.7500 0.01913(15) Uani d S 1 . .
Sm Sm2 0.0000 0.28693(2) 0.2500 0.01920(15) Uani d S 1 . .
O O1 0.0507(3) 0.1479(3) 0.5795(7) 0.0347(14) Uani d . 1 . .
O O2 0.0696(3) 0.2088(2) 0.3778(7) 0.0270(12) Uani d . 1 . .
O O3 0.0595(3) 0.2463(3) 0.0471(7) 0.0272(12) Uani d . 1 . .
O O4 0.0957(3) 0.1637(3) -0.0570(7) 0.0371(15) Uani d . 1 . .
O O5 0.0340(3) 0.3549(3) 0.4988(7) 0.0314(14) Uani d . 1 . .
O O6 0.0664(3) 0.2896(2) 0.7115(7) 0.0253(12) Uani d . 1 . .
C C1 0.0717(4) 0.1566(4) 0.4500(9) 0.0219(15) Uani d . 1 . .
C C2 0.0997(4) 0.1010(4) 0.3809(10) 0.0261(17) Uani d . 1 . .
C C3 0.0705(5) 0.0434(4) 0.3985(11) 0.038(2) Uani d . 1 . .
H H3A 0.0340 0.0418 0.4451 0.045 Uiso calc R 1 . .
C C4 0.0948(6) -0.0106(4) 0.3481(12) 0.047(3) Uani d . 1 . .
H H4A 0.0750 -0.0487 0.3608 0.056 Uiso calc R 1 . .
C C5 0.1484(6) -0.0084(5) 0.2790(11) 0.051(3) Uani d . 1 . .
H H5A 0.1650 -0.0448 0.2430 0.062 Uiso calc R 1 . .
C C6 0.1774(5) 0.0479(5) 0.2632(12) 0.043(2) Uani d . 1 . .
H H6A 0.2147 0.0484 0.2194 0.051 Uiso calc R 1 . .
C C7 0.1542(4) 0.1042(4) 0.3090(10) 0.0303(19) Uani d . 1 . .
C C8 0.1910(4) 0.1616(4) 0.2945(10) 0.0290(18) Uani d . 1 . .
C C9 0.2548(5) 0.1680(5) 0.3969(12) 0.043(2) Uani d . 1 . .
H H9A 0.2710 0.1377 0.4768 0.051 Uiso calc R 1 . .
C C10 0.2938(5) 0.2178(5) 0.3824(14) 0.049(3) Uani d . 1 . .
H H10A 0.3359 0.2209 0.4529 0.059 Uiso calc R 1 . .
C C11 0.2722(5) 0.2637(6) 0.2657(14) 0.047(3) Uani d . 1 . .
H H11A 0.2996 0.2971 0.2555 0.057 Uiso calc R 1 . .
C C12 0.2084(5) 0.2593(5) 0.1633(10) 0.037(2) Uani d . 1 . .
H H12A 0.1926 0.2902 0.0849 0.045 Uiso calc R 1 . .
C C13 0.1687(4) 0.2091(4) 0.1778(11) 0.0307(19) Uani d . 1 . .
C C14 0.1034(4) 0.2052(4) 0.0510(10) 0.0277(17) Uani d . 1 . .
C C15 0.0564(4) 0.3429(3) 0.6499(10) 0.0226(16) Uani d . 1 . .
C C16 0.0779(4) 0.3973(3) 0.7700(9) 0.0246(17) Uani d . 1 . .
C C17 0.1438(4) 0.3978(4) 0.8573(10) 0.0294(18) Uani d . 1 . .
H H17A 0.1715 0.3649 0.8458 0.035 Uiso calc R 1 . .
C C18 0.1689(5) 0.4476(5) 0.9620(12) 0.040(2) Uani d . 1 . .
H H18A 0.2131 0.4478 1.0206 0.048 Uiso calc R 1 . .
C C19 0.1282(5) 0.4962(4) 0.9784(11) 0.041(2) Uani d . 1 . .
H H19A 0.1452 0.5300 1.0458 0.049 Uiso calc R 1 . .
C C20 0.0622(5) 0.4954(4) 0.8956(11) 0.034(2) Uani d . 1 . .
H H20A 0.0348 0.5282 0.9097 0.041 Uiso calc R 1 . .
C C21 0.0358(5) 0.4454(3) 0.7900(10) 0.0278(18) Uani d . 1 . .
O O7 0.0919(4) 0.3610(3) 0.2356(8) 0.0474(18) Uani d . 1 . .
H H7B 0.1218 0.3708 0.3270 0.050 Uiso d . 1 . .
H H7A 0.1034 0.3561 0.1493 0.075 Uiso d . 1 . .
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'
Sm Sm -0.1638 3.4418 '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
_geom_angle_publ_flag
O1 Sm1 O1 2_556 . 114.5(3) ?
O1 Sm1 O6 2_556 . 150.4(2) ?
O1 Sm1 O6 . . 87.7(2) ?
O1 Sm1 O6 2_556 2_556 87.7(2) ?
O1 Sm1 O6 . 2_556 150.4(2) ?
O6 Sm1 O6 . 2_556 79.7(3) ?
O1 Sm1 O4 2_556 2 76.9(2) ?
O1 Sm1 O4 . 2 79.4(2) ?
O6 Sm1 O4 . 2 128.6(2) ?
O6 Sm1 O4 2_556 2 87.7(2) ?
O1 Sm1 O4 2_556 1_556 79.4(2) ?
O1 Sm1 O4 . 1_556 76.9(2) ?
O6 Sm1 O4 . 1_556 87.7(2) ?
O6 Sm1 O4 2_556 1_556 128.6(2) ?
O4 Sm1 O4 2 1_556 135.3(3) ?
O1 Sm1 O3 2_556 1_556 77.7(2) ?
O1 Sm1 O3 . 1_556 124.5(2) ?
O6 Sm1 O3 . 1_556 73.45(19) ?
O6 Sm1 O3 2_556 1_556 77.39(19) ?
O4 Sm1 O3 2 1_556 151.0(2) ?
O4 Sm1 O3 1_556 1_556 51.29(18) ?
O1 Sm1 O3 2_556 2 124.5(2) ?
O1 Sm1 O3 . 2 77.7(2) ?
O6 Sm1 O3 . 2 77.39(19) ?
O6 Sm1 O3 2_556 2 73.45(19) ?
O4 Sm1 O3 2 2 51.29(18) ?
O4 Sm1 O3 1_556 2 151.0(2) ?
O3 Sm1 O3 1_556 2 141.8(2) ?
O1 Sm1 C14 2_556 1_556 79.8(2) ?
O1 Sm1 C14 . 1_556 99.6(2) ?
O6 Sm1 C14 . 1_556 77.3(2) ?
O6 Sm1 C14 2_556 1_556 103.5(2) ?
O4 Sm1 C14 2 1_556 153.7(2) ?
O4 Sm1 C14 1_556 1_556 25.4(2) ?
O3 Sm1 C14 1_556 1_556 26.1(2) ?
O3 Sm1 C14 2 1_556 154.7(2) ?
O1 Sm1 C14 2_556 2 99.6(2) ?
O1 Sm1 C14 . 2 79.8(2) ?
O6 Sm1 C14 . 2 103.5(2) ?
O6 Sm1 C14 2_556 2 77.3(2) ?
O4 Sm1 C14 2 2 25.4(2) ?
O4 Sm1 C14 1_556 2 153.7(2) ?
O3 Sm1 C14 1_556 2 154.7(2) ?
O3 Sm1 C14 2 2 26.1(2) ?
C14 Sm1 C14 1_556 2 179.0(3) ?
O2 Sm2 O2 2 . 86.4(3) ?
O2 Sm2 O3 2 2 72.10(19) ?
O2 Sm2 O3 . 2 78.1(2) ?
O2 Sm2 O3 2 . 78.1(2) ?
O2 Sm2 O3 . . 72.10(19) ?
O3 Sm2 O3 2 . 138.7(3) ?
O2 Sm2 O5 2 . 146.3(2) ?
O2 Sm2 O5 . . 91.4(2) ?
O3 Sm2 O5 2 . 74.51(19) ?
O3 Sm2 O5 . . 132.9(2) ?
O2 Sm2 O5 2 2 91.4(2) ?
O2 Sm2 O5 . 2 146.3(2) ?
O3 Sm2 O5 2 2 132.9(2) ?
O3 Sm2 O5 . 2 74.51(19) ?
O5 Sm2 O5 . 2 108.0(3) ?
O2 Sm2 O7 2 . 147.4(2) ?
O2 Sm2 O7 . . 94.7(2) ?
O3 Sm2 O7 2 . 140.0(2) ?
O3 Sm2 O7 . . 71.3(2) ?
O5 Sm2 O7 . . 66.4(2) ?
O5 Sm2 O7 2 . 69.9(2) ?
O2 Sm2 O7 2 2 94.7(2) ?
O2 Sm2 O7 . 2 147.4(2) ?
O3 Sm2 O7 2 2 71.3(2) ?
O3 Sm2 O7 . 2 140.0(2) ?
O5 Sm2 O7 . 2 69.9(2) ?
O5 Sm2 O7 2 2 66.4(2) ?
O7 Sm2 O7 . 2 101.4(4) ?
C1 O1 Sm1 . . 137.2(5) ?
C1 O2 Sm2 . . 144.0(5) ?
C14 O3 Sm2 . . 134.8(5) ?
C14 O3 Sm1 . 1_554 88.3(5) ?
Sm2 O3 Sm1 . 1_554 123.6(2) ?
C14 O4 Sm1 . 1_554 98.4(5) ?
C15 O5 Sm2 . . 132.1(5) ?
C15 O6 Sm1 . . 135.5(5) ?
O2 C1 O1 . . 123.5(7) ?
O2 C1 C2 . . 119.8(7) ?
O1 C1 C2 . . 116.7(7) ?
C3 C2 C7 . . 120.1(8) ?
C3 C2 C1 . . 116.4(8) ?
C7 C2 C1 . . 123.4(7) ?
C4 C3 C2 . . 121.0(10) ?
C4 C3 H3A . . 119.5 ?
C2 C3 H3A . . 119.5 ?
C3 C4 C5 . . 119.7(10) ?
C3 C4 H4A . . 120.2 ?
C5 C4 H4A . . 120.2 ?
C6 C5 C4 . . 119.4(9) ?
C6 C5 H5A . . 120.3 ?
C4 C5 H5A . . 120.3 ?
C5 C6 C7 . . 123.5(11) ?
C5 C6 H6A . . 118.2 ?
C7 C6 H6A . . 118.2 ?
C6 C7 C2 . . 116.3(9) ?
C6 C7 C8 . . 119.1(9) ?
C2 C7 C8 . . 124.4(7) ?
C9 C8 C13 . . 117.0(9) ?
C9 C8 C7 . . 118.0(8) ?
C13 C8 C7 . . 124.9(7) ?
C10 C9 C8 . . 121.4(10) ?
C10 C9 H9A . . 119.3 ?
C8 C9 H9A . . 119.3 ?
C9 C10 C11 . . 121.5(9) ?
C9 C10 H10A . . 119.3 ?
C11 C10 H10A . . 119.3 ?
C10 C11 C12 . . 118.6(10) ?
C10 C11 H11A . . 120.7 ?
C12 C11 H11A . . 120.7 ?
C13 C12 C11 . . 120.2(10) ?
C13 C12 H12A . . 119.9 ?
C11 C12 H12A . . 119.9 ?
C12 C13 C8 . . 121.4(8) ?
C12 C13 C14 . . 116.2(8) ?
C8 C13 C14 . . 122.1(8) ?
O4 C14 O3 . . 120.9(8) ?
O4 C14 C13 . . 118.7(8) ?
O3 C14 C13 . . 120.2(7) ?
O4 C14 Sm1 . 1_554 56.2(4) ?
O3 C14 Sm1 . 1_554 65.5(4) ?
C13 C14 Sm1 . 1_554 164.9(6) ?
O6 C15 O5 . . 125.6(7) ?
O6 C15 C16 . . 116.1(7) ?
O5 C15 C16 . . 118.2(7) ?
C17 C16 C21 . . 120.2(7) ?
C17 C16 C15 . . 116.3(7) ?
C21 C16 C15 . . 123.5(7) ?
C16 C17 C18 . . 120.3(8) ?
C16 C17 H17A . . 119.9 ?
C18 C17 H17A . . 119.9 ?
C19 C18 C17 . . 119.8(9) ?
C19 C18 H18A . . 120.1 ?
C17 C18 H18A . . 120.1 ?
C18 C19 C20 . . 120.4(8) ?
C18 C19 H19A . . 119.8 ?
C20 C19 H19A . . 119.8 ?
C19 C20 C21 . . 120.7(9) ?
C19 C20 H20A . . 119.6 ?
C21 C20 H20A . . 119.6 ?
C16 C21 C20 . . 118.6(8) ?
C16 C21 C21 . 2_556 122.8(6) ?
C20 C21 C21 . 2_556 118.5(7) ?
Sm2 O7 H7B . . 119.9 ?
Sm2 O7 H7A . . 110.3 ?
H7B O7 H7A . . 119.3 ?
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
Sm1 O1 2_556 2.321(6) ?
Sm1 O1 . 2.321(6) ?
Sm1 O6 . 2.322(5) ?
Sm1 O6 2_556 2.322(5) ?
Sm1 O4 2 2.410(6) ?
Sm1 O4 1_556 2.410(6) ?
Sm1 O3 1_556 2.613(5) ?
Sm1 O3 2 2.613(5) ?
Sm1 C14 1_556 2.869(8) ?
Sm1 C14 2 2.869(8) ?
Sm2 O2 2 2.298(5) ?
Sm2 O2 . 2.298(5) ?
Sm2 O3 2 2.469(6) ?
Sm2 O3 . 2.469(6) ?
Sm2 O5 . 2.480(5) ?
Sm2 O5 2 2.480(5) ?
Sm2 O7 . 2.509(6) ?
Sm2 O7 2 2.509(6) ?
O1 C1 . 1.264(9) ?
O2 C1 . 1.263(9) ?
O3 C14 . 1.264(10) ?
O3 Sm1 1_554 2.613(5) ?
O4 C14 . 1.244(10) ?
O4 Sm1 1_554 2.410(6) ?
O5 C15 . 1.250(10) ?
O6 C15 . 1.248(9) ?
C1 C2 . 1.498(10) ?
C2 C3 . 1.399(12) ?
C2 C7 . 1.402(12) ?
C3 C4 . 1.369(13) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.370(16) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.370(15) ?
C5 H5A . 0.9300 ?
C6 C7 . 1.386(11) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.469(13) ?
C8 C9 . 1.397(12) ?
C8 C13 . 1.403(12) ?
C9 C10 . 1.362(15) ?
C9 H9A . 0.9300 ?
C10 C11 . 1.375(16) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.394(13) ?
C11 H11A . 0.9300 ?
C12 C13 . 1.377(13) ?
C12 H12A . 0.9300 ?
C13 C14 . 1.503(11) ?
C14 Sm1 1_554 2.869(8) ?
C15 C16 . 1.527(10) ?
C16 C17 . 1.387(12) ?
C16 C21 . 1.388(11) ?
C17 C18 . 1.394(12) ?
C17 H17A . 0.9300 ?
C18 C19 . 1.369(14) ?
C18 H18A . 0.9300 ?
C19 C20 . 1.376(14) ?
C19 H19A . 0.9300 ?
C20 C21 . 1.407(11) ?
C20 H20A . 0.9300 ?
C21 C21 2_556 1.477(18) ?
O7 H7B . 0.8798 ?
O7 H7A . 0.8122 ?
