#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:41:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180273 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/59/7115947.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_7115947
loop_
_publ_author_name
'Jane V. Knichal'
'William J. Gee'
'Andrew D. Burrows'
'Paul R. Raithby'
'Simon J. Teat'
'Chick C. Wilson'
_publ_section_title
;
 A facile single crystal to single crystal transition with significant
 structural contraction on desolvation
;
_journal_name_full               Chem.Commun.
_journal_page_first              14436
_journal_paper_doi               10.1039/C4cc06587E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C20 H8 O8 Pb2'
_chemical_formula_sum            'C20 H8 O8 Pb2'
_chemical_formula_weight         790.64
_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                100.148(3)
_cell_angle_beta                 91.407(3)
_cell_angle_gamma                107.941(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3790(4)
_cell_length_b                   10.0130(3)
_cell_length_c                   10.3180(4)
_cell_measurement_reflns_used    5621
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.58
_cell_measurement_theta_min      2.92
_cell_volume                     904.22(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'POV-Ray, version 3.6, 2004'
_computing_publication_material  'ENCIFER 4.1 (CCDC)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_sigmaI/netI    0.1217
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13225
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.58
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    18.645
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.4877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.821
_refine_diff_density_min         -2.454
_refine_diff_density_rms         0.327
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0122P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                3486
_reflns_number_total             5621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06587e2.cif
_cod_data_source_block           c:\bath1724
_cod_database_code               7115947
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 0.77693(5) 0.39552(4) 0.04164(4) 0.02338(12) Uani 1 1 d .
O1 O 0.9238(9) 0.5489(7) -0.1004(8) 0.0223(17) Uani 1 1 d .
C1 C 0.8629(12) 0.6462(10) -0.0650(11) 0.020(2) Uani 1 1 d .
Pb2 Pb 0.44295(5) 1.03023(4) -0.18227(4) 0.02540(13) Uani 1 1 d .
O2 O 0.7682(10) 0.6380(8) 0.0187(8) 0.0255(18) Uani 1 1 d .
C2 C 0.9027(12) 0.7736(10) -0.1319(11) 0.021(2) Uani 1 1 d .
O4 O 0.8673(9) 1.2387(7) -0.1242(7) 0.0226(16) Uani 1 1 d .
C3 C 0.8376(12) 0.8810(10) -0.0952(10) 0.018(2) Uani 1 1 d .
H3 H 0.7671 0.8717 -0.0301 0.022 Uiso 1 1 calc R
O3 O 0.6786(9) 1.0791(7) -0.0559(7) 0.0202(15) Uani 1 1 d .
C4 C 0.8741(13) 1.0004(10) -0.1520(11) 0.020(2) Uani 1 1 d .
O5 O 0.5519(9) 0.8910(8) -0.3267(8) 0.0259(17) Uani 1 1 d .
C5 C 0.9790(12) 1.0169(10) -0.2469(11) 0.019(2) Uani 1 1 d .
H5 H 1.0040 1.0994 -0.2860 0.023 Uiso 1 1 calc R
O6 O 0.4482(10) 0.7693(9) -0.1769(9) 0.035(2) Uani 1 1 d .
C6 C 1.0471(12) 0.9104(10) -0.2841(11) 0.020(2) Uani 1 1 d .
O7 O 0.5717(9) 0.3251(7) -0.1280(8) 0.0227(16) Uani 1 1 d .
C7 C 1.0080(12) 0.7894(10) -0.2264(10) 0.018(2) Uani 1 1 d .
H7 H 1.0534 0.7171 -0.2515 0.022 Uiso 1 1 calc R
O8 O 0.5730(10) 0.1891(8) -0.3224(8) 0.0288(19) Uani 1 1 d .
C8 C 1.1496(14) 0.9262(11) -0.3834(11) 0.025(2) Uani 1 1 d .
C9 C 1.2460(6) 0.9411(5) -0.4603(5) 0.035(3) Uani 1 1 d .
H9 H 1.3218 0.9528 -0.5207 0.042 Uiso 1 1 calc R
C10 C 0.8021(6) 1.1148(5) -0.1102(5) 0.019(2) Uani 1 1 d R
C11 C 0.5871(6) 0.3094(5) -0.2524(5) 0.018(2) Uani 1 1 d R
C12 C 0.6177(6) 0.4347(5) -0.3145(5) 0.034(3) Uani 1 1 d R
C13 C 0.5655(6) 0.5464(5) -0.2657(5) 0.023(2) Uani 1 1 d R
H13 H 0.5144 0.5442 -0.1873 0.027 Uiso 1 1 calc R
C14 C 0.5855(12) 0.6619(10) -0.3279(11) 0.019(2) Uani 1 1 d .
C15 C 0.6780(12) 0.6753(9) -0.4324(10) 0.019(2) Uani 1 1 d .
H15 H 0.6976 0.7572 -0.4720 0.023 Uiso 1 1 calc R
C16 C 0.7409(14) 0.5699(11) -0.4781(11) 0.027(3) Uani 1 1 d .
C17 C 0.7071(14) 0.4461(11) -0.4248(10) 0.024(2) Uani 1 1 d .
H17 H 0.7433 0.3700 -0.4614 0.029 Uiso 1 1 calc R
C18 C 0.8418(14) 0.5870(11) -0.5857(11) 0.025(2) Uani 1 1 d .
C19 C 0.9258(10) 0.6094(8) -0.6666(8) 0.030(3) Uani 1 1 d .
H19 H 0.9943 0.6276 -0.7326 0.036 Uiso 1 1 calc R
C20 C 0.5244(10) 0.7809(8) -0.2746(8) 0.022(2) Uani 1 1 d 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
O7 Pb1 O1 86.9(3) . .
O7 Pb1 O4 80.5(3) . 1_545
O1 Pb1 O4 73.8(2) . 1_545
O7 Pb1 O2 80.6(3) . .
O1 Pb1 O2 53.3(2) . .
O4 Pb1 O2 124.4(2) 1_545 .
O7 Pb1 O1 147.3(2) . 2_765
O1 Pb1 O1 69.5(3) . 2_765
O4 Pb1 O1 71.5(3) 1_545 2_765
O2 Pb1 O1 101.2(2) . 2_765
C1 O1 Pb1 92.7(6) . .
C1 O1 Pb1 120.0(6) . 2_765
Pb1 O1 Pb1 110.5(3) . 2_765
O2 C1 O1 123.1(8) . .
O2 C1 C2 118.6(9) . .
O1 C1 C2 118.2(9) . .
O5 Pb2 O3 80.5(3) . .
O5 Pb2 O8 76.1(2) . 1_565
O3 Pb2 O8 88.8(3) . 1_565
O5 Pb2 O6 52.0(2) . .
O3 Pb2 O6 78.5(3) . .
O8 Pb2 O6 127.8(3) 1_565 .
C1 O2 Pb1 90.8(6) . .
C3 C2 C7 119.1(9) . .
C3 C2 C1 119.3(9) . .
C7 C2 C1 121.5(9) . .
C10 O4 Pb1 106.1(5) . 1_565
C4 C3 C2 120.9(9) . .
C4 C3 H3 119.6 . .
C2 C3 H3 119.6 . .
C10 O3 Pb2 120.2(5) . .
C3 C4 C5 120.4(9) . .
C3 C4 C10 119.7(9) . .
C5 C4 C10 119.9(8) . .
C20 O5 Pb2 100.3(6) . .
C4 C5 C6 119.5(9) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
C20 O6 Pb2 86.2(5) . .
C7 C6 C5 119.4(9) . .
C7 C6 C8 121.6(10) . .
C5 C6 C8 119.0(9) . .
C11 O7 Pb1 124.5(5) . .
C6 C7 C2 120.7(9) . .
C6 C7 H7 119.6 . .
C2 C7 H7 119.6 . .
C11 O8 Pb2 101.5(5) . 1_545
C9 C8 C6 174.7(12) . .
C8 C9 H9 180.0 . .
O4 C10 O3 123.2(6) . .
O4 C10 C4 119.3(6) . .
O3 C10 C4 117.4(6) . .
O8 C11 O7 121.8(6) . .
O8 C11 C12 119.4(4) . .
O7 C11 C12 118.7(4) . .
C13 C12 C17 118.5(5) . .
C13 C12 C11 120.9 . .
C17 C12 C11 120.6(5) . .
C12 C13 C14 121.7(5) . .
C12 C13 H13 119.2 . .
C14 C13 H13 119.2 . .
C13 C14 C15 119.3(8) . .
C13 C14 C20 120.7(8) . .
C15 C14 C20 119.6(8) . .
C16 C15 C14 120.2(9) . .
C16 C15 H15 119.9 . .
C14 C15 H15 119.9 . .
C15 C16 C17 120.3(10) . .
C15 C16 C18 119.8(9) . .
C17 C16 C18 119.9(10) . .
C16 C17 C12 119.5(9) . .
C16 C17 H17 120.3 . .
C12 C17 H17 120.3 . .
C19 C18 C16 175.7(11) . .
C18 C19 H19 180.0 . .
O6 C20 O5 121.3(8) . .
O6 C20 C14 118.3(7) . .
O5 C20 C14 120.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O7 2.414(8) .
Pb1 O1 2.448(7) .
Pb1 O4 2.461(7) 1_545
Pb1 O2 2.506(7) .
Pb1 O1 2.719(8) 2_765
O1 C1 1.279(12) .
O1 Pb1 2.719(8) 2_765
C1 O2 1.248(13) .
C1 C2 1.508(13) .
Pb2 O5 2.330(8) .
Pb2 O3 2.407(8) .
Pb2 O8 2.410(7) 1_565
Pb2 O6 2.639(8) .
C2 C3 1.396(14) .
C2 C7 1.398(14) .
O4 C10 1.239(8) .
O4 Pb1 2.461(7) 1_565
C3 C4 1.377(13) .
C3 H3 0.9500 .
O3 C10 1.277(9) .
C4 C5 1.400(14) .
C4 C10 1.507(11) .
O5 C20 1.269(10) .
C5 C6 1.407(14) .
C5 H5 0.9500 .
O6 C20 1.252(11) .
C6 C7 1.396(12) .
C6 C8 1.419(15) .
O7 C11 1.283(9) .
C7 H7 0.9500 .
O8 C11 1.257(9) .
O8 Pb2 2.410(7) 1_545
C8 C9 1.209(13) .
C9 H9 0.9500 .
C11 C12 1.4620 .
C12 C13 1.3763 .
C12 C17 1.430(11) .
C13 C14 1.386(10) .
C13 H13 0.9500 .
C14 C15 1.399(14) .
C14 C20 1.503(12) .
C15 C16 1.380(15) .
C15 H15 0.9500 .
C16 C17 1.395(14) .
C16 C18 1.475(16) .
C17 H17 0.9500 .
C18 C19 1.166(14) .
C19 H19 0.9500 .
