#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:17:34 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179622 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/86/4508645.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4508645
loop_
_publ_author_name
'Xu, Xinxin'
'Lu, Ying'
'Wang, Enbo'
'Ma, Ying'
'Bai, Xiuli'
_publ_section_title
;
 Metal-Controlled Assembly of Coordination Polymers with the Flexible
 Ligand 1,1‘-Biphenyl-2,2‘-dicarboxylate Acid
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2029
_journal_paper_doi               10.1021/cg050671e
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C56 H32 O18 Pb6'
_chemical_formula_weight         2235.96
_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_method           SHELXL-97
_cell_angle_alpha                107.54(3)
_cell_angle_beta                 102.01(3)
_cell_angle_gamma                97.36(3)
_cell_formula_units_Z            1
_cell_length_a                   7.0119(14)
_cell_length_b                   13.788(3)
_cell_length_c                   14.968(3)
_cell_measurement_reflns_used    5682
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_volume                     1321.1(6)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12460
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         5682
_exptl_absorpt_coefficient_mu    19.125
_exptl_absorpt_correction_T_max  0.009
_exptl_absorpt_correction_T_min  0.005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.248
_refine_diff_density_max         2.215
_refine_diff_density_min         -2.324
_refine_diff_density_rms         0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1452
_reflns_number_gt                4601
_reflns_number_total             5682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050671esup1.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        1321.0(5)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4508645
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
Pb1 Pb 0.22201(5) 0.46900(3) 0.47123(3) 0.02272(13) Uani 1 1 d .
Pb2 Pb 0.48138(6) 0.51169(3) 0.28349(3) 0.02693(14) Uani 1 1 d .
Pb3 Pb 0.45962(6) 0.73146(3) 0.49091(3) 0.02723(14) Uani 1 1 d .
C28 C 0.7422(16) 0.7365(9) 0.7078(9) 0.030(3) Uani 1 1 d .
C21 C 0.6685(18) 0.8564(9) 0.8558(9) 0.031(3) Uani 1 1 d .
C13 C 0.9661(17) 0.5677(9) 0.3088(8) 0.028(2) Uani 1 1 d .
C23 C 0.9574(18) 0.7777(9) 0.8709(10) 0.032(3) Uani 1 1 d .
H23A H 1.0307 0.7319 0.8417 0.039 Uiso 1 1 calc R
O2 O 0.8418(11) 0.5483(6) 0.3530(6) 0.0275(16) Uani 1 1 d .
C24 C 1.018(2) 0.8286(11) 0.9704(11) 0.045(3) Uani 1 1 d .
H24A H 1.1346 0.8205 1.0076 0.054 Uiso 1 1 calc R
C22 C 0.7882(16) 0.7941(8) 0.8137(8) 0.025(2) Uani 1 1 d .
O11 O 0.6125(13) 0.3468(6) 0.2519(7) 0.037(2) Uani 1 1 d .
C26 C 0.727(2) 0.9063(9) 0.9564(9) 0.038(3) Uani 1 1 d .
H26A H 0.6492 0.9495 0.9857 0.045 Uiso 1 1 calc R
O10 O 0.5000(10) 0.5644(5) 0.4431(5) 0.0185(14) Uani 1 1 d .
O1 O 1.1493(11) 0.5839(7) 0.3453(6) 0.0313(18) Uani 1 1 d .
C16 C 0.3354(18) 0.8105(9) 0.7224(8) 0.030(2) Uani 1 1 d .
C15 C 0.489(2) 0.8821(9) 0.7993(9) 0.033(3) Uani 1 1 d .
C17 C 0.181(2) 0.8460(10) 0.6788(10) 0.040(3) Uani 1 1 d .
H17A H 0.0822 0.7987 0.6267 0.048 Uiso 1 1 calc R
C25 C 0.898(2) 0.8926(9) 1.0134(9) 0.040(3) Uani 1 1 d .
H25A H 0.9334 0.9260 1.0803 0.047 Uiso 1 1 calc R
O9 O 0.2851(13) 0.6504(6) 0.5972(6) 0.0355(19) Uani 1 1 d .
O4 O 0.7860(14) 0.7724(7) 0.4727(7) 0.042(2) Uani 1 1 d .
O8 O 0.6912(13) 0.7798(7) 0.6483(7) 0.038(2) Uani 1 1 d .
O3 O 0.6214(13) 0.7071(6) 0.3129(7) 0.0355(19) Uani 1 1 d .
O7 O 0.7565(14) 0.6411(7) 0.6840(7) 0.042(2) Uani 1 1 d .
C2 C 0.8957(16) 0.5746(10) 0.2088(7) 0.027(2) Uani 1 1 d .
C27 C 0.3376(16) 0.6969(10) 0.6905(8) 0.031(3) Uani 1 1 d .
C8 C 0.9597(19) 0.8018(9) 0.3641(9) 0.032(3) Uani 1 1 d .
C19 C 0.310(2) 1.0196(10) 0.7803(10) 0.039(3) Uani 1 1 d .
H19A H 0.3001 1.0890 0.7988 0.047 Uiso 1 1 calc R
C9 C 1.079(2) 0.8923(9) 0.4389(10) 0.035(3) Uani 1 1 d .
H9A H 1.0459 0.9138 0.4979 0.042 Uiso 1 1 calc R
C20 C 0.477(2) 0.9879(9) 0.8271(10) 0.036(3) Uani 1 1 d .
H20A H 0.5784 1.0371 0.8762 0.044 Uiso 1 1 calc R
C1 C 0.917(2) 0.6709(12) 0.1956(10) 0.044(3) Uani 1 1 d .
C14 C 0.771(2) 0.7534(10) 0.3816(10) 0.037(3) Uani 1 1 d .
C3 C 0.809(2) 0.4836(12) 0.1322(9) 0.043(3) Uani 1 1 d .
H3A H 0.7881 0.4204 0.1425 0.051 Uiso 1 1 calc R
C4 C 0.755(2) 0.4887(13) 0.0386(10) 0.055(4) Uani 1 1 d .
H4A H 0.7032 0.4281 -0.0147 0.066 Uiso 1 1 calc R
C6 C 0.856(3) 0.6731(16) 0.1025(12) 0.063(5) Uani 1 1 d .
H6A H 0.8669 0.7368 0.0925 0.075 Uiso 1 1 calc R
C7 C 1.016(2) 0.7663(10) 0.2780(10) 0.039(3) Uani 1 1 d .
C11 C 1.298(2) 0.9147(11) 0.3414(12) 0.048(4) Uani 1 1 d .
H11A H 1.4097 0.9521 0.3336 0.057 Uiso 1 1 calc R
C10 C 1.243(2) 0.9497(11) 0.4268(13) 0.050(4) Uani 1 1 d .
H10A H 1.3143 1.0109 0.4756 0.060 Uiso 1 1 calc R
C18 C 0.166(2) 0.9454(11) 0.7075(11) 0.046(3) Uani 1 1 d .
H18A H 0.0548 0.9647 0.6773 0.055 Uiso 1 1 calc R
C12 C 1.192(2) 0.8261(14) 0.2677(12) 0.057(4) Uani 1 1 d .
H12A H 1.2320 0.8041 0.2108 0.069 Uiso 1 1 calc R
C5 C 0.779(3) 0.5847(15) 0.0257(12) 0.063(5) Uani 1 1 d .
H5A H 0.7420 0.5883 -0.0365 0.076 Uiso 1 1 calc R
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'
Pb Pb -3.3944 10.1111 '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
O10 Pb1 O10 73.8(3) 2_666 .
O10 Pb1 O7 94.5(3) 2_666 2_666
O10 Pb1 O7 76.8(3) . 2_666
O10 Pb1 O9 90.6(3) 2_666 .
O10 Pb1 O9 75.8(2) . .
O7 Pb1 O9 149.5(3) 2_666 .
O10 Pb1 Pb1 132.83(17) 2_666 2_566
O10 Pb1 Pb1 133.70(16) . 2_566
O7 Pb1 Pb1 125.3(2) 2_666 2_566
O9 Pb1 Pb1 68.3(2) . 2_566
O10 Pb1 Pb3 95.25(17) 2_666 .
O10 Pb1 Pb3 36.67(16) . .
O7 Pb1 Pb3 104.4(2) 2_666 .
O9 Pb1 Pb3 45.10(19) . .
Pb1 Pb1 Pb3 97.50(3) 2_566 .
O10 Pb2 O2 78.9(2) . .
O10 Pb2 O11 104.5(3) . .
O2 Pb2 O11 69.1(3) . .
O10 Pb2 O3 85.5(3) . .
O2 Pb2 O3 71.7(3) . .
O11 Pb2 O3 136.5(3) . .
O10 Pb2 O7 72.7(3) . 2_666
O2 Pb2 O7 119.4(3) . 2_666
O11 Pb2 O7 68.1(3) . 2_666
O3 Pb2 O7 151.8(3) . 2_666
O10 Pb2 Pb3 35.83(17) . .
O2 Pb2 Pb3 87.57(18) . .
O11 Pb2 Pb3 138.9(2) . .
O3 Pb2 Pb3 55.0(2) . .
O7 Pb2 Pb3 97.96(17) 2_666 .
O10 Pb3 O4 84.8(3) . .
O10 Pb3 O8 94.4(3) . .
O4 Pb3 O8 72.1(3) . .
O10 Pb3 O9 76.8(2) . .
O4 Pb3 O9 138.4(3) . .
O8 Pb3 O9 72.5(3) . .
O10 Pb3 Pb2 35.42(18) . .
O4 Pb3 Pb2 75.9(2) . .
O8 Pb3 Pb2 122.2(2) . .
O9 Pb3 Pb2 105.92(17) . .
O10 Pb3 Pb1 39.00(17) . .
O4 Pb3 Pb1 123.2(2) . .
O8 Pb3 Pb1 98.9(2) . .
O9 Pb3 Pb1 43.95(17) . .
Pb2 Pb3 Pb1 62.11(3) . .
O8 C28 O7 123.5(11) . .
O8 C28 C22 120.7(11) . .
O7 C28 C22 115.8(11) . .
C22 C21 C26 118.3(12) . .
C22 C21 C15 124.2(11) . .
C26 C21 C15 117.3(10) . .
O2 C13 O1 122.1(10) . .
O2 C13 C2 119.7(10) . .
O1 C13 C2 118.2(9) . .
C24 C23 C22 121.2(11) . .
C13 O2 Pb2 123.5(7) . .
C23 C24 C25 118.3(13) . .
C21 C22 C23 120.7(11) . .
C21 C22 C28 123.4(11) . .
C23 C22 C28 115.8(9) . .
C27 O11 Pb2 126.9(8) 2_666 .
C25 C26 C21 121.2(12) . .
Pb2 O10 Pb3 108.8(3) . .
Pb2 O10 Pb1 111.2(3) . 2_666
Pb3 O10 Pb1 116.3(3) . 2_666
Pb2 O10 Pb1 109.7(3) . .
Pb3 O10 Pb1 104.3(2) . .
Pb1 O10 Pb1 106.2(3) 2_666 .
C17 C16 C15 118.9(11) . .
C17 C16 C27 120.3(12) . .
C15 C16 C27 120.8(10) . .
C16 C15 C20 118.3(12) . .
C16 C15 C21 125.9(10) . .
C20 C15 C21 115.9(12) . .
C18 C17 C16 122.8(14) . .
C26 C25 C24 120.2(12) . .
C27 O9 Pb1 140.4(8) . .
C27 O9 Pb3 118.3(8) . .
Pb1 O9 Pb3 91.0(2) . .
C14 O4 Pb3 107.6(8) . .
C28 O8 Pb3 136.1(8) . .
C14 O3 Pb2 118.1(7) . .
C28 O7 Pb1 127.1(8) . 2_666
C28 O7 Pb2 125.0(7) . 2_666
Pb1 O7 Pb2 94.7(3) 2_666 2_666
C3 C2 C1 121.6(12) . .
C3 C2 C13 118.1(12) . .
C1 C2 C13 120.3(11) . .
O11 C27 O9 123.4(12) 2_666 .
O11 C27 C16 121.9(10) 2_666 .
O9 C27 C16 114.7(11) . .
C7 C8 C9 118.9(12) . .
C7 C8 C14 124.1(12) . .
C9 C8 C14 116.9(11) . .
C18 C19 C20 118.2(11) . .
C10 C9 C8 122.0(12) . .
C15 C20 C19 120.1(12) . .
C6 C1 C2 118.1(15) . .
C6 C1 C7 121.3(15) . .
C2 C1 C7 120.4(11) . .
O3 C14 O4 127.3(12) . .
O3 C14 C8 120.8(11) . .
O4 C14 C8 111.7(12) . .
C2 C3 C4 118.5(15) . .
C5 C4 C3 119.6(14) . .
C5 C6 C1 121.4(17) . .
C8 C7 C12 118.2(13) . .
C8 C7 C1 126.1(13) . .
C12 C7 C1 115.7(13) . .
C10 C11 C12 121.5(13) . .
C11 C10 C9 119.0(14) . .
C17 C18 C19 121.6(13) . .
C11 C12 C7 120.4(13) . .
C6 C5 C4 120.7(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O10 2.281(7) 2_666
Pb1 O10 2.393(7) .
Pb1 O7 2.409(8) 2_666
Pb1 O9 2.557(8) .
Pb1 Pb1 3.5383(11) 2_566
Pb1 Pb3 3.6833(12) .
Pb2 O10 2.248(7) .
Pb2 O2 2.447(8) .
Pb2 O11 2.511(8) .
Pb2 O3 2.616(8) .
Pb2 O7 2.741(9) 2_666
Pb2 Pb3 3.6726(15) .
Pb3 O10 2.270(7) .
Pb3 O4 2.377(9) .
Pb3 O8 2.411(9) .
Pb3 O9 2.609(9) .
C28 O8 1.233(15) .
C28 O7 1.278(14) .
C28 C22 1.487(16) .
C21 C22 1.385(15) .
C21 C26 1.398(16) .
C21 C15 1.512(18) .
C13 O2 1.247(13) .
C13 O1 1.249(13) .
C13 C2 1.512(15) .
C23 C24 1.385(19) .
C23 C22 1.397(17) .
C24 C25 1.405(18) .
O11 C27 1.214(15) 2_666
C26 C25 1.39(2) .
O10 Pb1 2.281(7) 2_666
C16 C17 1.369(17) .
C16 C15 1.407(18) .
C16 C27 1.496(17) .
C15 C20 1.409(16) .
C17 C18 1.332(18) .
O9 C27 1.296(14) .
O4 C14 1.286(16) .
O3 C14 1.245(16) .
O7 Pb1 2.409(8) 2_666
O7 Pb2 2.741(9) 2_666
C2 C3 1.380(18) .
C2 C1 1.394(19) .
C27 O11 1.214(15) 2_666
C8 C7 1.393(18) .
C8 C9 1.418(18) .
C8 C14 1.512(17) .
C19 C18 1.36(2) .
C19 C20 1.421(19) .
C9 C10 1.386(19) .
C1 C6 1.381(19) .
C1 C7 1.47(2) .
C3 C4 1.40(2) .
C4 C5 1.39(2) .
C6 C5 1.35(3) .
C7 C12 1.45(2) .
C11 C10 1.38(2) .
C11 C12 1.37(2) .
