#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:25:04 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179059 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/21/4302113.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_4302113
loop_
_publ_author_name
'Monika Plabst'
'Thomas Bein'
_publ_contact_author             'Bein, Thomas'
_publ_contact_author_email       tbein@cup.uni-muenchen.de
_publ_section_title
;
1,4-Phenylenebis(methylidyne)tetrakis(phosphonic acid): A New Building
Block in Metal Organic Framework Synthesis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4331
_journal_page_last               4341
_journal_paper_doi               10.1021/ic802294e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         La2[(HO3P)(O3P)-CH-C6H4-CH-(PO3)(PO3H)].8H2O
_chemical_formula_sum            'C8 H24 La2 O20 P4'
_chemical_formula_weight         841.97
_chemical_name_common            La2(H2L)
_chemical_name_systematic
;
 ?
;
_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_date             2008-10-04T00:11:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                99.7269(15)
_cell_angle_beta                 103.6343(14)
_cell_angle_gamma                107.8791(14)
_cell_formula_units_Z            1
_cell_length_a                   6.2659(2)
_cell_length_b                   9.8383(2)
_cell_length_c                   10.4758(2)
_cell_measurement_reflns_used    11955
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     576.59(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.1078574
_diffrn_orient_matrix_UB_12      -0.0528127
_diffrn_orient_matrix_UB_13      0.030748
_diffrn_orient_matrix_UB_21      -0.0712688
_diffrn_orient_matrix_UB_22      -0.0749226
_diffrn_orient_matrix_UB_23      -0.0902522
_diffrn_orient_matrix_UB_31      0.1196909
_diffrn_orient_matrix_UB_32      0.0619454
_diffrn_orient_matrix_UB_33      -0.035529
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12625
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    4.023
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2638
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0139
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0100P)²+0.8117P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0334
_refine_ls_wR_factor_ref         0.0337
_reflns_number_gt                2570
_reflns_number_total             2638
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802294e_si_002.cif
_cod_data_source_block           ln097
_cod_original_cell_volume        576.59(2)
_cod_database_code               4302113
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La La -0.236800(18) 0.477658(11) 0.157853(10) 0.00731(4) Uani 1 1 d . . .
P1 P 0.40165(8) 0.62413(5) 0.23185(5) 0.00738(9) Uani 1 1 d . . .
P2 P 0.17603(9) 0.80940(5) 0.09752(5) 0.00862(10) Uani 1 1 d . . .
O1 O 0.1855(2) 0.54987(15) 0.27249(14) 0.0120(3) Uani 1 1 d . . .
O2 O -0.0510(2) 0.72194(15) 0.12023(14) 0.0130(3) Uani 1 1 d . . .
O3 O 0.6294(2) 0.62389(15) 0.32471(13) 0.0112(3) Uani 1 1 d . . .
O4 O 0.3853(2) 0.55039(15) 0.08640(13) 0.0108(3) Uani 1 1 d . . .
O5 O 0.1973(3) 0.97368(15) 0.11039(15) 0.0129(3) Uani 1 1 d D . .
O6 O 0.1966(3) 0.75044(16) -0.04028(14) 0.0144(3) Uani 1 1 d . . .
O7 O -0.6196(3) 0.26677(17) 0.10490(17) 0.0206(3) Uani 1 1 d D . .
O9 O 0.0389(3) 0.90816(19) -0.22026(16) 0.0218(3) Uani 1 1 d D . .
O8 O -0.2367(4) 0.3614(2) 0.3636(2) 0.0340(4) Uani 1 1 d D . .
O10 O 0.6851(4) 0.6683(2) 0.59384(17) 0.0324(4) Uani 1 1 d D . .
C1 C 0.4235(3) 0.8131(2) 0.23153(19) 0.0087(3) Uani 1 1 d . . .
C2 C 0.4583(3) 0.9086(2) 0.37037(19) 0.0097(4) Uani 1 1 d . . .
C3 C 0.2734(4) 0.9057(2) 0.4236(2) 0.0147(4) Uani 1 1 d . . .
C4 C 0.6837(4) 1.0037(2) 0.4487(2) 0.0137(4) Uani 1 1 d . . .
H1 H 0.558(6) 0.853(4) 0.203(3) 0.043(3) Uiso 1 1 d . . .
H3 H 0.118(6) 0.844(4) 0.374(3) 0.043(3) Uiso 1 1 d . . .
H4 H 0.807(6) 1.008(4) 0.414(3) 0.043(3) Uiso 1 1 d . . .
H5 H 0.113(5) 1.003(3) 0.148(3) 0.043(3) Uiso 1 1 d D . .
H91 H 0.101(5) 0.870(3) -0.166(3) 0.043(3) Uiso 1 1 d D . .
H92 H -0.059(4) 0.838(2) -0.282(2) 0.043(3) Uiso 1 1 d D . .
H71 H -0.721(4) 0.267(4) 0.039(2) 0.043(3) Uiso 1 1 d D . .
H72 H -0.635(6) 0.1797(12) 0.097(3) 0.043(3) Uiso 1 1 d D . .
H102 H 0.693(6) 0.659(3) 0.5158(13) 0.043(3) Uiso 1 1 d D . .
H101 H 0.722(6) 0.601(2) 0.618(3) 0.043(3) Uiso 1 1 d D . .
H81 H -0.363(3) 0.339(4) 0.380(3) 0.043(3) Uiso 1 1 d D . .
H82 H -0.112(3) 0.379(4) 0.422(3) 0.043(3) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.015
0 1 0 0.035
0 0 1 0.035
0 0 -1 0.025
1 0 0 0.08
-1 0 0 0.04
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 La O1 120.97(5) 2_565 . ?
O4 La O2 73.81(5) 2_565 . ?
O1 La O2 74.83(4) . . ?
O4 La O6 73.05(4) 2_565 2_565 ?
O1 La O6 83.77(5) . 2_565 ?
O2 La O6 122.35(5) . 2_565 ?
O4 La O7 81.21(5) 2_565 . ?
O1 La O7 140.81(5) . . ?
O2 La O7 144.28(5) . . ?
O6 La O7 71.89(5) 2_565 . ?
O4 La O3 120.81(4) 2_565 1_455 ?
O1 La O3 103.39(4) . 1_455 ?
O2 La O3 83.34(5) . 1_455 ?
O6 La O3 154.24(5) 2_565 1_455 ?
O7 La O3 88.13(5) . 1_455 ?
O4 La O8 148.85(6) 2_565 . ?
O1 La O8 77.94(6) . . ?
O2 La O8 137.32(6) . . ?
O6 La O8 86.00(6) 2_565 . ?
O7 La O8 70.32(6) . . ?
O3 La O8 71.73(5) 1_455 . ?
O4 La O4 66.33(5) 2_565 1_455 ?
O1 La O4 149.95(4) . 1_455 ?
O2 La O4 80.48(4) . 1_455 ?
O6 La O4 124.54(4) 2_565 1_455 ?
O7 La O4 66.11(5) . 1_455 ?
O3 La O4 56.30(4) 1_455 1_455 ?
O8 La O4 110.86(5) . 1_455 ?
O4 La P1 94.32(3) 2_565 1_455 ?
O1 La P1 129.02(3) . 1_455 ?
O2 La P1 82.49(3) . 1_455 ?
O6 La P1 145.24(4) 2_565 1_455 ?
O7 La P1 74.26(4) . 1_455 ?
O3 La P1 27.86(3) 1_455 1_455 ?
O8 La P1 89.98(4) . 1_455 ?
O4 La P1 28.53(3) 1_455 1_455 ?
O1 P1 O3 113.04(8) . . ?
O1 P1 O4 113.05(8) . . ?
O3 P1 O4 106.16(8) . . ?
O1 P1 C1 108.72(8) . . ?
O3 P1 C1 110.24(8) . . ?
O4 P1 C1 105.34(8) . . ?
O1 P1 La 126.51(6) . 1_655 ?
O3 P1 La 50.77(5) . 1_655 ?
O4 P1 La 55.61(5) . 1_655 ?
C1 P1 La 124.77(6) . 1_655 ?
O6 P2 O2 113.79(8) . . ?
O6 P2 O5 107.42(8) . . ?
O2 P2 O5 110.15(8) . . ?
O6 P2 C1 110.04(8) . . ?
O2 P2 C1 108.88(8) . . ?
O5 P2 C1 106.28(8) . . ?
P1 O1 La 131.79(8) . . ?
P2 O2 La 138.67(8) . . ?
P1 O3 La 101.37(7) . 1_655 ?
P1 O4 La 148.29(8) . 2_565 ?
P1 O4 La 95.86(6) . 1_655 ?
La O4 La 113.67(5) 2_565 1_655 ?
P2 O5 H5 117(2) . . ?
P2 O6 La 135.94(8) . 2_565 ?
La O7 H71 112(2) . . ?
La O7 H72 125(2) . . ?
H71 O7 H72 106(3) . . ?
H91 O9 H92 105(3) . . ?
La O8 H81 114(2) . . ?
La O8 H82 119(2) . . ?
H81 O8 H82 122(3) . . ?
H102 O10 H101 104.2(12) . . ?
C2 C1 P2 114.15(13) . . ?
C2 C1 P1 113.51(13) . . ?
P2 C1 P1 109.36(10) . . ?
C2 C1 H1 109(2) . . ?
P2 C1 H1 104.8(19) . . ?
P1 C1 H1 105.1(19) . . ?
C4 C2 C3 117.92(18) . . ?
C4 C2 C1 119.06(17) . . ?
C3 C2 C1 123.02(18) . . ?
C4 C3 C2 120.37(19) 2_676 . ?
C4 C3 H3 118(2) 2_676 . ?
C2 C3 H3 121(2) . . ?
C2 C4 C3 121.72(19) . 2_676 ?
C2 C4 H4 119(2) . . ?
C3 C4 H4 119(2) 2_676 . ?
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
La O4 2.4435(13) 2_565 ?
La O1 2.4514(14) . ?
La O2 2.4709(14) . ?
La O6 2.4851(14) 2_565 ?
La O7 2.5086(15) . ?
La O3 2.5316(13) 1_455 ?
La O8 2.6055(17) . ?
La O4 2.6578(13) 1_455 ?
La P1 3.2038(5) 1_455 ?
P1 O1 1.5225(14) . ?
P1 O3 1.5271(14) . ?
P1 O4 1.5381(13) . ?
P1 C1 1.8219(19) . ?
P1 La 3.2038(5) 1_655 ?
P2 O6 1.5125(14) . ?
P2 O2 1.5156(15) . ?
P2 O5 1.5601(14) . ?
P2 C1 1.8162(19) . ?
O3 La 2.5316(13) 1_655 ?
O4 La 2.4435(13) 2_565 ?
O4 La 2.6578(13) 1_655 ?
O5 H5 0.820(5) . ?
O6 La 2.4851(14) 2_565 ?
O7 H71 0.821(5) . ?
O7 H72 0.820(5) . ?
O9 H91 0.820(5) . ?
O9 H92 0.821(5) . ?
O8 H81 0.820(5) . ?
O8 H82 0.818(5) . ?
O10 H102 0.822(5) . ?
O10 H101 0.822(5) . ?
C1 C2 1.519(3) . ?
C1 H1 0.96(3) . ?
C2 C4 1.388(3) . ?
C2 C3 1.394(3) . ?
C3 C4 1.392(3) 2_676 ?
C3 H3 0.94(3) . ?
C4 C3 1.392(3) 2_676 ?
C4 H4 0.92(3) . ?
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
O5 H5 O9 0.820(5) 1.694(8) 2.505(2) 170(3) 2_575
O9 H91 O6 0.820(5) 2.016(8) 2.827(2) 170(3) .
O9 H92 O10 0.821(5) 1.921(8) 2.734(3) 170(3) 1_454
O7 H71 O2 0.821(5) 1.968(6) 2.788(2) 177(3) 2_465
O7 H72 O5 0.820(5) 2.021(16) 2.773(2) 152(3) 1_445
O10 H102 O3 0.822(5) 1.895(9) 2.700(2) 166(3) .
O10 H101 O1 0.822(5) 2.156(8) 2.962(2) 167(2) 2_666
O8 H81 O10 0.820(5) 2.081(10) 2.882(3) 165(3) 2_566
O8 H82 O1 0.818(5) 3.01(3) 3.183(2) 94(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 P1 O1 La -170.20(9) . . . . ?
O4 P1 O1 La -49.55(12) . . . . ?
C1 P1 O1 La 67.05(12) . . . . ?
La P1 O1 La -112.89(8) 1_655 . . . ?
O4 La O1 P1 19.20(13) 2_565 . . . ?
O2 La O1 P1 -40.83(10) . . . . ?
O6 La O1 P1 85.14(11) 2_565 . . . ?
O7 La O1 P1 136.18(10) . . . . ?
O3 La O1 P1 -119.99(10) 1_455 . . . ?
O8 La O1 P1 172.37(12) . . . . ?
O4 La O1 P1 -76.66(14) 1_455 . . . ?
P1 La O1 P1 -107.63(10) 1_455 . . . ?
O6 P2 O2 La 70.90(14) . . . . ?
O5 P2 O2 La -168.41(11) . . . . ?
C1 P2 O2 La -52.23(14) . . . . ?
O4 La O2 P2 -94.76(13) 2_565 . . . ?
O1 La O2 P2 34.57(12) . . . . ?
O6 La O2 P2 -37.67(14) 2_565 . . . ?
O7 La O2 P2 -142.19(11) . . . . ?
O3 La O2 P2 140.43(13) 1_455 . . . ?
O8 La O2 P2 86.74(14) . . . . ?
O4 La O2 P2 -162.72(13) 1_455 . . . ?
P1 La O2 P2 168.50(12) 1_455 . . . ?
O1 P1 O3 La 119.17(7) . . . 1_655 ?
O4 P1 O3 La -5.31(8) . . . 1_655 ?
C1 P1 O3 La -118.92(8) . . . 1_655 ?
O1 P1 O4 La 81.41(17) . . . 2_565 ?
O3 P1 O4 La -154.10(14) . . . 2_565 ?
C1 P1 O4 La -37.16(18) . . . 2_565 ?
La P1 O4 La -159.09(18) 1_655 . . 2_565 ?
O1 P1 O4 La -119.50(7) . . . 1_655 ?
O3 P1 O4 La 4.99(8) . . . 1_655 ?
C1 P1 O4 La 121.93(7) . . . 1_655 ?
O2 P2 O6 La -66.85(14) . . . 2_565 ?
O5 P2 O6 La 170.94(11) . . . 2_565 ?
C1 P2 O6 La 55.64(14) . . . 2_565 ?
O6 P2 C1 C2 163.70(13) . . . . ?
O2 P2 C1 C2 -70.95(15) . . . . ?
O5 P2 C1 C2 47.68(15) . . . . ?
O6 P2 C1 P1 -67.92(12) . . . . ?
O2 P2 C1 P1 57.43(12) . . . . ?
O5 P2 C1 P1 176.07(9) . . . . ?
O1 P1 C1 C2 62.52(15) . . . . ?
O3 P1 C1 C2 -61.92(15) . . . . ?
O4 P1 C1 C2 -176.05(13) . . . . ?
La P1 C1 C2 -117.55(12) 1_655 . . . ?
O1 P1 C1 P2 -66.22(11) . . . . ?
O3 P1 C1 P2 169.35(9) . . . . ?
O4 P1 C1 P2 55.22(11) . . . . ?
La P1 C1 P2 113.72(8) 1_655 . . . ?
P2 C1 C2 C4 -134.86(17) . . . . ?
P1 C1 C2 C4 98.90(19) . . . . ?
P2 C1 C2 C3 45.0(2) . . . . ?
P1 C1 C2 C3 -81.3(2) . . . . ?
C4 C2 C3 C4 0.0(3) . . . 2_676 ?
C1 C2 C3 C4 -179.78(18) . . . 2_676 ?
C3 C2 C4 C3 0.0(3) . . . 2_676 ?
C1 C2 C4 C3 179.79(19) . . . 2_676 ?
