#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/02/2200209.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_2200209
loop_
_publ_author_name
'Shi, Qian'
'Hu, Maolin'
'Cao, Rong'
'Liang, Yucang'
'Hong, Maochun'
_publ_section_title
Tetra-μ-benzoato-O:O'-bis[(benzoato-O,O')(1,10-phenanthroline-N,N')lanthanum(III)]
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m122
_journal_page_last               m123
_journal_paper_doi               10.1107/S1600536801002963
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[La2 (C7 H5 O2)6 (C12 H8 N2)2]'
_chemical_formula_moiety         'C66 H46 La2 N4 O12'
_chemical_formula_sum            'C66 H46 La2 N4 O12'
_chemical_formula_weight         1364.92
_chemical_name_systematic
;
Tetra-μ-benzoato-O:O'-bis[(benzoato-O,O')(1,10-phenanthroline-N,N')-
lanthanum(III)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                104.8880(10)
_cell_angle_beta                 93.2680(10)
_cell_angle_gamma                113.4020(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9356(2)
_cell_length_b                   11.9818(2)
_cell_length_c                   12.4945(3)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      1.71
_cell_volume                     1428.49(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        SMART
_computing_molecular_graphics    SHELXL97
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .972
_diffrn_measured_fraction_theta_max .972
_diffrn_measurement_device       'Siemens Smart CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0185
_diffrn_reflns_av_sigmaI/netI    .0369
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7321
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.544
_exptl_absorpt_correction_T_max  .734
_exptl_absorpt_correction_T_min  .546
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plane
_exptl_crystal_F_000             679
_exptl_crystal_size_max          .31
_exptl_crystal_size_mid          .21
_exptl_crystal_size_min          .20
_refine_diff_density_max         .614
_refine_diff_density_min         -.593
_refine_ls_extinction_coef       .0022(4)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          .0280
_refine_ls_R_factor_gt           .0237
_refine_ls_shift/su_max          .017
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0302P)²+0.0941P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0597
_reflns_number_gt                4427
_reflns_number_total             4901
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ob6029.cif
_cod_data_source_block           I
_cod_original_cell_volume        1428.48(5)
_cod_database_code               2200209
_cod_database_fobs_code          2200209
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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
_atom_site_type_symbol
La -.135359(14) -.064305(13) -.147434(12) .03130(7) Uani d . 1 . . La
O1 -.1594(2) .14151(19) -.06398(19) .0532(6) Uani d . 1 . . O
O2 -.00697(19) .14069(18) .05750(17) .0420(5) Uani d . 1 . . O
O3 -.24532(19) -.13991(19) .00349(17) .0444(5) Uani d . 1 . . O
O4 -.09329(19) -.09061(19) .15456(17) .0469(5) Uani d . 1 . . O
O5 -.0776(2) -.18940(18) -.32531(17) .0470(5) Uani d . 1 . . O
O6 -.27652(19) -.28549(18) -.27926(17) .0465(5) Uani d . 1 . . O
N1 -.1939(2) .0122(2) -.3216(2) .0414(5) Uani d . 1 . . N
N2 -.3883(2) -.0725(2) -.1963(2) .0392(5) Uani d . 1 . . N
C1 -.1033(3) .0481(3) -.3865(3) .0499(7) Uani d . 1 . . C
H1 -.0300 .0274 -.3826 .060 Uiso calc R 1 . . H
C2 -.1123(4) .1156(3) -.4605(3) .0578(9) Uani d . 1 . . C
H2 -.0485 .1361 -.5068 .069 Uiso calc R 1 . . H
C3 -.2159(4) .1506(3) -.4635(3) .0581(9) Uani d . 1 . . C
H3 -.2212 .1988 -.5097 .070 Uiso calc R 1 . . H
C4 -.3144(3) .1146(3) -.3973(3) .0485(7) Uani d . 1 . . C
C5 -.4279(4) .1459(3) -.3971(3) .0612(9) Uani d . 1 . . C
H5 -.4353 .1964 -.4402 .073 Uiso calc R 1 . . H
C6 -.5232(4) .1043(3) -.3364(3) .0616(9) Uani d . 1 . . C
H6 -.5959 .1259 -.3384 .074 Uiso calc R 1 . . H
C7 -.5155(3) .0267(3) -.2683(3) .0468(7) Uani d . 1 . . C
C8 -.6144(3) -.0214(3) -.2047(3) .0568(9) Uani d . 1 . . C
H8 -.6912 -.0059 -.2077 .068 Uiso calc R 1 . . H
C9 -.5985(3) -.0902(3) -.1392(3) .0547(8) Uani d . 1 . . C
H9 -.6631 -.1213 -.0961 .066 Uiso calc R 1 . . H
C10 -.4830(3) -.1140(3) -.1375(3) .0481(7) Uani d . 1 . . C
H10 -.4728 -.1616 -.0923 .058 Uiso calc R 1 . . H
C11 -.4034(3) -.0023(3) -.2620(2) .0385(6) Uani d . 1 . . C
C12 -.3009(3) .0423(3) -.3277(2) .0398(6) Uani d . 1 . . C
C25 -.0702(3) .1973(3) .0226(2) .0367(6) Uani d . 1 . . C
C26 -.0376(3) .3331(2) .0848(2) .0365(6) Uani d . 1 . . C
C27 -.1281(3) .3832(3) .0642(3) .0476(7) Uani d . 1 . . C
H27 -.2096 .3313 .0145 .057 Uiso calc R 1 . . H
C28 -.0972(4) .5099(3) .1173(3) .0587(9) Uani d . 1 . . C
H28 -.1587 .5429 .1048 .070 Uiso calc R 1 . . H
C29 .0246(4) .5869(3) .1887(3) .0632(10) Uani d . 1 . . C
H29 .0458 .6725 .2235 .076 Uiso calc R 1 . . H
C30 .1146(4) .5389(3) .2091(3) .0605(9) Uani d . 1 . . C
H30 .1969 .5920 .2574 .073 Uiso calc R 1 . . H
C31 .0839(3) .4112(3) .1578(3) .0471(7) Uani d . 1 . . C
H31 .1449 .3783 .1725 .057 Uiso calc R 1 . . H
C32 -.2088(3) -.1552(2) .0936(2) .0370(6) Uani d . 1 . . C
C33 -.3104(3) -.2564(2) .1341(2) .0377(6) Uani d . 1 . . C
C34 -.4448(3) -.3183(3) .0809(3) .0550(8) Uani d . 1 . . C
H34 -.4724 -.2972 .0202 .066 Uiso calc R 1 . . H
C35 -.5378(4) -.4113(4) .1178(3) .0698(11) Uani d . 1 . . C
H35 -.6279 -.4518 .0819 .084 Uiso calc R 1 . . H
C36 -.4993(4) -.4443(3) .2060(3) .0671(10) Uani d . 1 . . C
H36 -.5623 -.5083 .2293 .081 Uiso calc R 1 . . H
C37 -.3676(4) -.3829(3) .2601(3) .0650(10) Uani d . 1 . . C
H37 -.3412 -.4049 .3207 .078 Uiso calc R 1 . . H
C38 -.2730(3) -.2881(3) .2254(3) .0500(8) Uani d . 1 . . C
H38 -.1839 -.2458 .2638 .060 Uiso calc R 1 . . H
C39 -.1889(3) -.2858(3) -.3417(2) .0376(6) Uani d . 1 . . C
C40 -.2195(3) -.4036(3) -.4372(2) .0392(6) Uani d . 1 . . C
C41 -.1209(4) -.4147(3) -.4977(3) .0545(8) Uani d . 1 . . C
H41 -.0335 -.3495 -.4777 .065 Uiso calc R 1 . . H
C42 -.1520(5) -.5227(4) -.5882(3) .0714(11) Uani d . 1 . . C
H42 -.0853 -.5303 -.6284 .086 Uiso calc R 1 . . H
C43 -.2805(5) -.6179(4) -.6181(3) .0759(12) Uani d . 1 . . C
H43 -.3011 -.6897 -.6794 .091 Uiso calc R 1 . . H
C44 -.3795(4) -.6087(3) -.5587(3) .0670(10) Uani d . 1 . . C
H44 -.4671 -.6735 -.5800 .080 Uiso calc R 1 . . H
C45 -.3483(3) -.5025(3) -.4670(3) .0495(7) Uani d . 1 . . C
H45 -.4145 -.4974 -.4250 .059 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -.2871 2.4523 '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
O2 La O3 2 . 72.52(7) yes
O2 La O4 2 2 79.10(7) yes
O3 La O4 . 2 134.26(7) yes
O2 La O6 2 . 91.19(7) yes
O3 La O6 . . 87.38(7) yes
O4 La O6 2 . 128.87(6) yes
O2 La O1 2 . 126.03(7) yes
O3 La O1 . . 87.45(7) yes
O4 La O1 2 . 81.04(7) yes
O6 La O1 . . 138.47(7) yes
O2 La O5 2 . 80.24(7) yes
O3 La O5 . . 129.53(7) yes
O4 La O5 2 . 77.79(6) yes
O6 La O5 . . 51.07(6) yes
O1 La O5 . . 141.97(7) yes
O2 La N1 2 . 148.16(7) yes
O3 La N1 . . 138.33(7) yes
O4 La N1 2 . 79.48(7) yes
O6 La N1 . . 84.22(7) yes
O1 La N1 . . 72.91(7) yes
O5 La N1 . . 72.40(7) yes
O2 La N2 2 . 148.23(7) yes
O3 La N2 . . 78.28(7) yes
O4 La N2 2 . 131.77(7) yes
O6 La N2 . . 75.01(7) yes
O1 La N2 . . 63.59(7) yes
O5 La N2 . . 110.24(7) yes
N1 La N2 . . 60.11(7) yes
O2 La O2 2 . 78.60(6) yes
O3 La O2 . . 73.34(6) yes
O4 La O2 2 . 66.31(6) yes
O6 La O2 . . 160.12(7) yes
O1 La O2 . . 47.49(6) yes
O5 La O2 . . 141.02(6) yes
N1 La O2 . . 113.37(6) yes
N2 La O2 . . 104.95(6) yes
C25 O1 La . . 103.24(17) no
C25 O2 La . 2 170.92(18) no
C25 O2 La . . 87.49(16) no
La O2 La 2 . 101.40(6) yes
C32 O3 La . . 136.59(17) no
C32 O4 La . 2 139.76(18) no
C39 O5 La . . 91.70(16) no
C39 O6 La . . 95.59(16) no
C1 N1 C12 . . 118.2(3) no
C1 N1 La . . 120.1(2) no
C12 N1 La . . 119.95(18) no
C10 N2 C11 . . 118.1(3) no
C10 N2 La . . 121.6(2) no
C11 N2 La . . 118.13(17) no
N1 C1 C2 . . 123.3(3) no
C3 C2 C1 . . 118.8(3) no
C2 C3 C4 . . 120.2(3) no
C3 C4 C12 . . 117.6(3) no
C3 C4 C5 . . 123.5(3) no
C12 C4 C5 . . 118.8(3) no
C6 C5 C4 . . 121.5(3) no
C5 C6 C7 . . 121.2(3) no
C11 C7 C8 . . 117.1(3) no
C11 C7 C6 . . 119.5(3) no
C8 C7 C6 . . 123.3(3) no
C9 C8 C7 . . 120.3(3) no
C8 C9 C10 . . 118.8(3) no
N2 C10 C9 . . 123.4(3) no
N2 C11 C7 . . 122.4(3) no
N2 C11 C12 . . 118.4(3) no
C7 C11 C12 . . 119.3(3) no
N1 C12 C4 . . 121.8(3) no
N1 C12 C11 . . 118.5(3) no
C4 C12 C11 . . 119.6(3) no
O1 C25 O2 . . 121.0(2) no
O1 C25 C26 . . 118.8(3) no
O2 C25 C26 . . 120.2(3) no
C31 C26 C27 . . 119.5(3) no
C31 C26 C25 . . 121.1(3) no
C27 C26 C25 . . 119.3(3) no
C28 C27 C26 . . 120.1(3) no
C29 C28 C27 . . 119.8(3) no
C30 C29 C28 . . 120.6(3) no
C29 C30 C31 . . 120.2(3) no
C26 C31 C30 . . 119.7(3) no
O3 C32 O4 . . 124.9(2) no
O3 C32 C33 . . 118.2(2) no
O4 C32 C33 . . 116.9(3) no
C38 C33 C34 . . 118.5(3) no
C38 C33 C32 . . 121.2(3) no
C34 C33 C32 . . 120.3(3) no
C35 C34 C33 . . 120.3(3) no
C36 C35 C34 . . 120.8(3) no
C35 C36 C37 . . 119.6(3) no
C36 C37 C38 . . 120.6(3) no
C33 C38 C37 . . 120.2(3) no
O5 C39 O6 . . 121.6(2) no
O5 C39 C40 . . 119.5(3) no
O6 C39 C40 . . 118.9(2) no
C41 C40 C45 . . 119.1(3) no
C41 C40 C39 . . 120.8(3) no
C45 C40 C39 . . 120.1(3) no
C40 C41 C42 . . 120.1(3) no
C43 C42 C41 . . 120.0(4) no
C42 C43 C44 . . 120.6(3) no
C43 C44 C45 . . 119.6(4) no
C44 C45 C40 . . 120.6(3) no
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
La O2 2 2.4460(19) yes
La O3 . 2.4685(19) yes
La O4 2 2.4756(18) yes
La O6 . 2.5173(19) yes
La O1 . 2.542(2) yes
La O5 . 2.6048(19) yes
La N1 . 2.704(2) yes
La N2 . 2.756(2) yes
La O2 . 2.860(2) yes
O1 C25 . 1.249(3) no
O2 C25 . 1.272(3) no
O2 La 2 2.4460(19) no
O3 C32 . 1.255(4) no
O4 C32 . 1.259(3) no
O4 La 2 2.4756(18) no
O5 C39 . 1.262(3) no
O6 C39 . 1.270(3) no
N1 C1 . 1.325(4) no
N1 C12 . 1.358(4) no
N2 C10 . 1.314(4) no
N2 C11 . 1.363(4) no
C1 C2 . 1.399(5) no
C2 C3 . 1.357(5) no
C3 C4 . 1.395(5) no
C4 C12 . 1.416(4) no
C4 C5 . 1.432(5) no
C5 C6 . 1.334(5) no
C6 C7 . 1.433(5) no
C7 C11 . 1.404(4) no
C7 C8 . 1.404(5) no
C8 C9 . 1.351(5) no
C9 C10 . 1.402(5) no
C11 C12 . 1.438(4) no
C25 C26 . 1.495(4) no
C26 C31 . 1.382(4) no
C26 C27 . 1.388(4) no
C27 C28 . 1.382(4) no
C28 C29 . 1.373(5) no
C29 C30 . 1.364(5) no
C30 C31 . 1.389(4) no
C32 C33 . 1.506(4) no
C33 C38 . 1.382(4) no
C33 C34 . 1.386(4) no
C34 C35 . 1.379(4) no
C35 C36 . 1.361(6) no
C36 C37 . 1.365(5) no
C37 C38 . 1.385(4) no
C39 C40 . 1.498(4) no
C40 C41 . 1.380(4) no
C40 C45 . 1.383(4) no
C41 C42 . 1.388(5) no
C42 C43 . 1.364(6) no
C43 C44 . 1.371(6) no
C44 C45 . 1.382(4) no
