#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/17/8101772.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_8101772
loop_
_publ_author_name
'Li, X.'
'Wang, D.-Y.'
'Hu, H.-M.'
_publ_section_title
;
Crystal structure of diaquabis(1,10-phenanthroline)-dilanthanum(III) 
tris(μ-1,4-benzenedicarboxylate), La₂(H₂O)₂(C₁₂H₈N₂)
₂(C₈H₄O₄)₃
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              271
_journal_page_last               272
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety         La~2~(H~2~O)~2~(phen)~2~(bdc)~3~
_chemical_formula_structural     La2(H2O)2(C12H8N2)2(C8H4O4)3
_chemical_formula_sum            'C24 H16 La N2 O7'
_chemical_formula_weight         583.30
_chemical_name_systematic
; 
diaquabis(1,10-phenanthroline)lanthanum(III) tris(1,4-benzenedicarboxylate)
;
_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                109.435(6)
_cell_angle_beta                 92.016(4)
_cell_angle_gamma                112.162(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4236(12)
_cell_length_b                   10.8499(9)
_cell_length_c                   11.4483(15)
_cell_measurement_reflns_used    3824
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.6
_cell_volume                     1111.5(2)
_computing_cell_refinement       'RAPID AUTO (Rigaku,2001)'
_computing_data_collection       'RAPID AUTO (Rigaku,2001)'
_computing_data_reduction        'RAPID AUTO (Rigaku,2001)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXTL (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku R-axis RAPID IP''
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotate anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3824
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.971
_exptl_absorpt_correction_T_max  0.7699
_exptl_absorpt_correction_T_min  0.6084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0135(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         3824
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0292
_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)+(0.0309P)²+3.1263P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                3677
_reflns_number_total             3824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1523.cff
_cod_data_source_block           51
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101772
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.58492(2) 0.49161(2) 0.334117(18) 0.02499(10) Uani 1 2 i d . . .
N1 N 0.6190(4) 0.3106(4) 0.1232(3) 0.0448(9) Uani 1 2 i d . . .
N2 N 0.8464(4) 0.5004(4) 0.3068(4) 0.0512(10) Uani 1 2 i d . . .
O1 O 0.3358(3) 0.3047(3) 0.2626(3) 0.0526(8) Uani 1 2 i d . . .
O1W O 0.4529(3) 0.5087(4) 0.1486(3) 0.0512(8) Uani 1 2 i d D . .
O3 O -0.3150(4) -0.3022(4) 0.0945(3) 0.0685(12) Uani 1 2 i d . . .
O4 O -0.2672(3) -0.3016(3) 0.2843(3) 0.0396(7) Uani 1 2 i d . . .
O5 O 0.6058(4) 0.2884(4) 0.3794(4) 0.0638(10) Uani 1 2 i d . . .
C1 C 0.2591(4) 0.2792(4) 0.3392(4) 0.0420(10) Uani 1 2 i d . . .
C2 C 0.1311(4) 0.1411(4) 0.2986(3) 0.0296(8) Uani 1 2 i d . . .
C3 C 0.0354(5) 0.0930(5) 0.1899(4) 0.0446(11) Uani 1 2 i d . . .
H3A H 0.0525 0.1447 0.1373 0.053 Uiso 1 2 i calc R . .
C4 C -0.0857(4) -0.0316(5) 0.1585(4) 0.0427(10) Uani 1 2 i d . . .
H4A H -0.1513 -0.0610 0.0869 0.051 Uiso 1 2 i calc R . .
C5 C -0.1103(4) -0.1131(4) 0.2328(3) 0.0298(8) Uani 1 2 i d . . .
C6 C -0.2399(4) -0.2493(4) 0.2002(4) 0.0348(8) Uani 1 2 i d . . .
C7 C -0.0110(4) -0.0669(5) 0.3389(4) 0.0409(10) Uani 1 2 i d . . .
H7A H -0.0246 -0.1218 0.3885 0.049 Uiso 1 2 i calc R . .
C8 C 0.1080(4) 0.0596(5) 0.3720(4) 0.0406(10) Uani 1 2 i d . . .
H8A H 0.1730 0.0901 0.4444 0.049 Uiso 1 2 i calc R . .
C9 C 0.5549(4) 0.2685(5) 0.4709(5) 0.0458(11) Uani 1 2 i d . . .
C10 C 0.5278(4) 0.1304(4) 0.4880(4) 0.0301(8) Uani 1 2 i d . . .
C11 C 0.4447(5) 0.0907(4) 0.5720(4) 0.0415(10) Uani 1 2 i d . . .
H11A H 0.4073 0.1516 0.6207 0.050 Uiso 1 2 i calc R . .
C12 C 0.5829(5) 0.0390(4) 0.4161(4) 0.0382(9) Uani 1 2 i d . . .
H12A H 0.6389 0.0650 0.3594 0.046 Uiso 1 2 i calc R . .
C13 C 0.5071(7) 0.2105(7) 0.0372(5) 0.0735(17) Uani 1 2 i d . . .
H13A H 0.4182 0.2004 0.0553 0.088 Uiso 1 2 i calc R . .
C14 C 0.5153(11) 0.1204(11) -0.0777(7) 0.129(4) Uani 1 2 i d . . .
H14A H 0.4339 0.0510 -0.1347 0.155 Uiso 1 2 i calc R . .
C15 C 0.6401(13) 0.1345(12) -0.1050(7) 0.134(4) Uani 1 2 i d . . .
H15A H 0.6463 0.0753 -0.1828 0.161 Uiso 1 2 i calc R . .
C16 C 0.7647(10) 0.2371(10) -0.0195(7) 0.097(3) Uani 1 2 i d . . .
C17 C 0.8979(13) 0.2548(15) -0.0431(9) 0.133(4) Uani 1 2 i d . . .
H17A H 0.9082 0.1990 -0.1207 0.160 Uiso 1 2 i calc R . .
C18 C 1.0123(10) 0.3502(12) 0.0431(10) 0.117(4) Uani 1 2 i d . . .
H18A H 1.1006 0.3615 0.0228 0.141 Uiso 1 2 i calc R . .
C19 C 1.0039(7) 0.4378(9) 0.1685(9) 0.089(2) Uani 1 2 i d . . .
C20 C 1.1139(9) 0.5293(12) 0.2606(14) 0.130(4) Uani 1 2 i d . . .
H20A H 1.2041 0.5402 0.2462 0.156 Uiso 1 2 i calc R . .
C21 C 1.0976(7) 0.6086(9) 0.3768(12) 0.125(4) Uani 1 2 i d . . .
H21A H 1.1750 0.6723 0.4407 0.150 Uiso 1 2 i calc R . .
C22 C 0.9570(6) 0.5893(7) 0.3956(8) 0.085(2) Uani 1 2 i d . . .
H22A H 0.9439 0.6417 0.4733 0.102 Uiso 1 2 i calc R . .
C23 C 0.8679(6) 0.4235(6) 0.1934(6) 0.0573(14) Uani 1 2 i d . . .
C24 C 0.7481(6) 0.3231(6) 0.0980(5) 0.0561(13) Uani 1 2 i d . . .
O2 O 0.2809(6) 0.3628(4) 0.4512(3) 0.1010(19) Uani 1 2 i d . . .
O6 O 0.5245(5) 0.3576(4) 0.5484(6) 0.116(2) Uani 1 2 i d . . .
H1WA H 0.513(5) 0.562(6) 0.122(6) 0.080 Uiso 1 2 i d D . .
H1WB H 0.403(6) 0.446(5) 0.084(4) 0.080 Uiso 1 2 i 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'
N N 0.0061 0.0033 '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'
La La -0.2871 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 La1 O2 69.2(2) 2_666 2_666 ?
O6 La1 O4 86.43(12) 2_666 1_665 ?
O2 La1 O4 84.70(11) 2_666 1_665 ?
O6 La1 O5 125.57(16) 2_666 . ?
O2 La1 O5 84.27(14) 2_666 . ?
O4 La1 O5 138.81(12) 1_665 . ?
O6 La1 O1 83.22(15) 2_666 . ?
O2 La1 O1 129.09(14) 2_666 . ?
O4 La1 O1 136.72(10) 1_665 . ?
O5 La1 O1 78.16(12) . . ?
O6 La1 O1W 80.8(2) 2_666 . ?
O2 La1 O1W 141.26(14) 2_666 . ?
O4 La1 O1W 69.06(9) 1_665 . ?
O5 La1 O1W 134.13(12) . . ?
O1 La1 O1W 67.83(10) . . ?
O6 La1 N1 154.11(19) 2_666 . ?
O2 La1 N1 136.14(17) 2_666 . ?
O4 La1 N1 90.62(11) 1_665 . ?
O5 La1 N1 71.06(12) . . ?
O1 La1 N1 81.40(12) . . ?
O1W La1 N1 74.14(12) . . ?
O6 La1 N2 139.81(16) 2_666 . ?
O2 La1 N2 78.02(18) 2_666 . ?
O4 La1 N2 67.57(11) 1_665 . ?
O5 La1 N2 71.34(12) . . ?
O1 La1 N2 136.66(12) . . ?
O1W La1 N2 114.63(12) . . ?
N1 La1 N2 60.15(12) . . ?
O6 La1 La1 49.08(14) 2_666 2_666 ?
O2 La1 La1 55.06(13) 2_666 2_666 ?
O4 La1 La1 126.23(7) 1_665 2_666 ?
O5 La1 La1 76.62(10) . 2_666 ?
O1 La1 La1 74.40(8) . 2_666 ?
O1W La1 La1 119.81(9) . 2_666 ?
N1 La1 La1 142.86(8) . 2_666 ?
N2 La1 La1 125.02(9) . 2_666 ?
O6 La1 La1 34.64(6) . 2_666 ?
O2 La1 La1 35.43(6) . 2_666 ?
C13 N1 C24 118.2(4) . . ?
C13 N1 La1 119.8(4) . . ?
C24 N1 La1 121.9(3) . . ?
C22 N2 C23 117.9(5) . . ?
C22 N2 La1 121.5(4) . . ?
C23 N2 La1 120.1(3) . . ?
C1 O1 La1 121.3(3) . . ?
La1 O1W H1WA 106(5) . . ?
La1 O1W H1WB 130(5) . . ?
H1WA O1W H1WB 102(6) . . ?
C6 O4 La1 146.2(3) . 1_445 ?
C9 O5 La1 114.5(3) . . ?
O1 C1 O2 124.2(4) . . ?
O1 C1 C2 119.4(4) . . ?
O2 C1 C2 116.4(4) . . ?
C8 C2 C3 119.2(3) . . ?
C8 C2 C1 118.9(3) . . ?
C3 C2 C1 121.9(3) . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
C3 C4 C5 120.6(4) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C7 C5 C4 118.5(3) . . ?
C7 C5 C6 119.9(3) . . ?
C4 C5 C6 121.7(3) . . ?
O3 C6 O4 124.0(4) . . ?
O3 C6 C5 118.8(3) . . ?
O4 C6 C5 117.1(3) . . ?
C8 C7 C5 120.8(4) . . ?
C8 C7 H7A 119.6 . . ?
C5 C7 H7A 119.6 . . ?
C2 C8 C7 120.4(4) . . ?
C2 C8 H8A 119.8 . . ?
C7 C8 H8A 119.8 . . ?
O6 C9 O5 122.4(5) . . ?
O6 C9 C10 118.3(5) . . ?
O5 C9 C10 119.3(4) . . ?
C11 C10 C12 119.4(4) . . ?
C11 C10 C9 121.0(4) . . ?
C12 C10 C9 119.6(4) . . ?
C12 C11 C10 120.4(4) 2_656 . ?
C12 C11 H11A 119.8 2_656 . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C10 120.3(4) 2_656 . ?
C11 C12 H12A 119.9 2_656 . ?
C10 C12 H12A 119.9 . . ?
N1 C13 C14 123.6(7) . . ?
N1 C13 H13A 118.2 . . ?
C14 C13 H13A 118.2 . . ?
C15 C14 C13 118.8(8) . . ?
C15 C14 H14A 120.6 . . ?
C13 C14 H14A 120.6 . . ?
C14 C15 C16 121.6(6) . . ?
C14 C15 H15A 119.2 . . ?
C16 C15 H15A 119.2 . . ?
C17 C16 C15 123.8(8) . . ?
C17 C16 C24 119.7(9) . . ?
C15 C16 C24 116.4(7) . . ?
C18 C17 C16 121.3(8) . . ?
C18 C17 H17A 119.4 . . ?
C16 C17 H17A 119.4 . . ?
C17 C18 C19 122.3(7) . . ?
C17 C18 H18A 118.9 . . ?
C19 C18 H18A 118.9 . . ?
C20 C19 C23 117.8(8) . . ?
C20 C19 C18 125.0(7) . . ?
C23 C19 C18 117.2(8) . . ?
C19 C20 C21 121.7(7) . . ?
C19 C20 H20A 119.1 . . ?
C21 C20 H20A 119.1 . . ?
C20 C21 C22 117.6(7) . . ?
C20 C21 H21A 121.2 . . ?
C22 C21 H21A 121.2 . . ?
N2 C22 C21 122.3(8) . . ?
N2 C22 H22A 118.9 . . ?
C21 C22 H22A 118.9 . . ?
N2 C23 C19 122.7(6) . . ?
N2 C23 C24 118.3(4) . . ?
C19 C23 C24 119.0(6) . . ?
N1 C24 C16 121.2(6) . . ?
N1 C24 C23 118.3(4) . . ?
C16 C24 C23 120.4(6) . . ?
C1 O2 La1 155.5(5) . 2_666 ?
C1 O2 La1 73.1(3) . . ?
La1 O2 La1 89.51(14) 2_666 . ?
C9 O6 La1 166.8(5) . 2_666 ?
C9 O6 La1 79.6(4) . . ?
La1 O6 La1 96.28(16) 2_666 . ?
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
La1 O6 2.416(4) 2_666 ?
La1 O2 2.449(3) 2_666 ?
La1 O4 2.458(2) 1_665 ?
La1 O5 2.509(3) . ?
La1 O1 2.510(3) . ?
La1 O1W 2.586(3) . ?
La1 N1 2.691(3) . ?
La1 N2 2.723(4) . ?
La1 O6 3.212(6) . ?
La1 O2 3.463(5) . ?
La1 La1 4.2249(6) 2_666 ?
N1 C13 1.327(7) . ?
N1 C24 1.353(6) . ?
N2 C22 1.311(7) . ?
N2 C23 1.369(7) . ?
O1 C1 1.236(5) . ?
O1W H1WA 0.82(2) . ?
O1W H1WB 0.81(2) . ?
O3 C6 1.240(5) . ?
O4 C6 1.261(5) . ?
O4 La1 2.458(2) 1_445 ?
O5 C9 1.237(6) . ?
C1 O2 1.253(6) . ?
C1 C2 1.492(5) . ?
C2 C8 1.376(5) . ?
C2 C3 1.380(5) . ?
C3 C4 1.381(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.384(5) . ?
C4 H4A 0.9300 . ?
C5 C7 1.383(5) . ?
C5 C6 1.496(5) . ?
C7 C8 1.379(6) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 O6 1.226(6) . ?
C9 C10 1.497(5) . ?
C10 C11 1.383(5) . ?
C10 C12 1.383(5) . ?
C11 C12 1.381(6) 2_656 ?
C11 H11A 0.9300 . ?
C12 C11 1.381(6) 2_656 ?
C12 H12A 0.9300 . ?
C13 C14 1.381(8) . ?
C13 H13A 0.9300 . ?
C14 C15 1.313(13) . ?
C14 H14A 0.9300 . ?
C15 C16 1.406(13) . ?
C15 H15A 0.9300 . ?
C16 C17 1.378(12) . ?
C16 C24 1.419(8) . ?
C17 C18 1.331(14) . ?
C17 H17A 0.9300 . ?
C18 C19 1.461(12) . ?
C18 H18A 0.9300 . ?
C19 C20 1.331(14) . ?
C19 C23 1.417(7) . ?
C20 C21 1.380(14) . ?
C20 H20A 0.9300 . ?
C21 C22 1.435(11) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C24 1.422(8) . ?
O2 La1 2.449(3) 2_666 ?
O6 La1 2.416(4) 2_666 ?
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
O1W H1WA O3 0.82(2) 1.96(2) 2.767(4) 167(6) 1_665
O1W H1WB O3 0.81(2) 2.03(2) 2.823(5) 167(7) 2
