#------------------------------------------------------------------------------
#$Date: 2019-11-25 02:21:40 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239955 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/05/4350597.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_4350597
loop_
_publ_author_name
'Zhang, Zhang-Jing'
'Guo, Guo-Cong'
'Xu, Gang'
'Fu, Ming-Lai'
'Zou, Jian-Ping'
'Huang, Jin-Shun'
_publ_section_title
;
 [(H2en)7(C2O4)2]n(Pb4I18)n.4nH2O, a new type of perovskite co-templated
 by both organic cations and anions.
;
_journal_issue                   25
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10028
_journal_page_last               10030
_journal_paper_doi               10.1021/ic061555j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C9 H39 I9 N7 O6 Pb2'
_chemical_formula_weight         1897.95
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                105.314(2)
_cell_angle_beta                 112.061(2)
_cell_angle_gamma                104.900(2)
_cell_formula_units_Z            2
_cell_length_a                   12.083(4)
_cell_length_b                   13.678(4)
_cell_length_c                   14.004(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1897.4(11)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_publication_material  'Siemens SHELXTLTM 5'
_computing_structure_refinement  'Siemens SHELXTLTM 5'
_computing_structure_solution    'Siemens SHELXTLTM 5'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14255
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    16.216
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1662
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.477
_refine_diff_density_min         -1.482
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6448
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                5500
_reflns_number_total             6448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061555jsi20060816_104930.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1897.3(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4350597
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 -0.074530(13) 1.092285(12) 0.213847(11) 0.01423(4) Uani 1 1 d .
Pb2 Pb 0.228158(13) 0.781070(12) 0.378955(11) 0.01469(4) Uani 1 1 d .
I1 I -0.21968(2) 1.21367(2) 0.09698(2) 0.02028(8) Uani 1 1 d .
I2 I -0.14263(2) 1.16236(2) 0.413726(18) 0.01640(8) Uani 1 1 d .
I3 I 0.19476(2) 1.29854(2) 0.37036(2) 0.02248(9) Uani 1 1 d .
I4 I -0.34234(2) 0.88515(2) 0.09795(2) 0.01857(8) Uani 1 1 d .
I5 I 0.07871(2) 0.94034(2) 0.305510(19) 0.01758(8) Uani 1 1 d .
I6 I 0.0000 1.0000 0.0000 0.01880(11) Uani 1 2 d S
I7 I -0.03048(2) 0.57229(2) 0.23156(2) 0.01766(8) Uani 1 1 d .
I8 I 0.29059(2) 0.72028(2) 0.182871(19) 0.01883(8) Uani 1 1 d .
I9 I 0.37652(2) 0.65551(2) 0.492530(19) 0.01718(8) Uani 1 1 d .
I10 I 0.5000 1.0000 0.5000 0.02203(12) Uani 1 2 d S
C1 C -0.1165(4) 0.5886(4) -0.0746(4) 0.0292(14) Uani 1 1 d U
H1D H -0.1540 0.5472 -0.0399 0.035 Uiso 1 1 calc R
H1E H -0.0435 0.5709 -0.0738 0.035 Uiso 1 1 calc R
C2 C -0.0685(4) 0.7051(4) -0.0075(3) 0.0279(14) Uani 1 1 d U
H2D H -0.0400 0.7467 -0.0464 0.033 Uiso 1 1 calc R
H2E H 0.0067 0.7247 0.0635 0.033 Uiso 1 1 calc R
C3 C 0.5278(3) 0.9667(4) 0.7808(3) 0.0278(15) Uani 1 1 d .
H3D H 0.5266 1.0398 0.8017 0.033 Uiso 1 1 calc R
H3E H 0.4670 0.9248 0.7012 0.033 Uiso 1 1 calc R
C4 C 0.6608(3) 0.9769(3) 0.8004(3) 0.0192(12) Uani 1 1 d U
H4D H 0.7175 1.0043 0.8807 0.023 Uiso 1 1 calc R
H4E H 0.6939 1.0310 0.7744 0.023 Uiso 1 1 calc R
C5 C 0.8056(4) 0.8331(3) 0.3902(3) 0.0223(13) Uani 1 1 d .
H5D H 0.8526 0.8942 0.3788 0.027 Uiso 1 1 calc R
H5E H 0.8522 0.8467 0.4691 0.027 Uiso 1 1 calc R
C6 C 0.6699(3) 0.8299(3) 0.3627(3) 0.0216(13) Uani 1 1 d .
H6D H 0.6772 0.9026 0.4035 0.026 Uiso 1 1 calc R
H6E H 0.6210 0.8115 0.2829 0.026 Uiso 1 1 calc R
C7 C -0.0675(3) 0.5030(3) 0.4773(3) 0.0186(12) Uani 1 1 d .
H7D H -0.1036 0.4952 0.5274 0.022 Uiso 1 1 calc R
H7E H -0.0594 0.5738 0.4726 0.022 Uiso 1 1 calc R
C11 C 0.5524(3) 0.4760(3) 0.2564(3) 0.0163(12) Uani 1 1 d .
C21 C 0.4917(4) 0.3506(4) 0.2181(3) 0.0322(15) Uani 1 1 d .
N1 N -0.2168(3) 0.5510(3) -0.1950(3) 0.0350(13) Uani 1 1 d .
H1A H -0.2438 0.4783 -0.2304 0.052 Uiso 1 1 calc R
H1B H -0.1819 0.5853 -0.2290 0.052 Uiso 1 1 calc R
H1C H -0.2842 0.5672 -0.1968 0.052 Uiso 1 1 calc R
N2 N -0.1647(3) 0.7370(3) 0.0151(3) 0.0300(13) Uani 1 1 d .
H2A H -0.1306 0.8096 0.0552 0.045 Uiso 1 1 calc R
H2B H -0.1885 0.7017 0.0537 0.045 Uiso 1 1 calc R
H2C H -0.2340 0.7194 -0.0497 0.045 Uiso 1 1 calc R
N3 N 0.4861(3) 0.9131(3) 0.8439(3) 0.0336(13) Uani 1 1 d .
H3A H 0.4062 0.9084 0.8297 0.050 Uiso 1 1 calc R
H3B H 0.5406 0.9521 0.9171 0.050 Uiso 1 1 calc R
H3C H 0.4856 0.8455 0.8241 0.050 Uiso 1 1 calc R
N4 N 0.6660(3) 0.8710(3) 0.7429(3) 0.0250(12) Uani 1 1 d .
H4A H 0.7479 0.8822 0.7585 0.037 Uiso 1 1 calc R
H4B H 0.6167 0.8466 0.6688 0.037 Uiso 1 1 calc R
H4C H 0.6366 0.8211 0.7669 0.037 Uiso 1 1 calc R
N5 N 0.8044(3) 0.7297(3) 0.3211(3) 0.0243(11) Uani 1 1 d .
H5A H 0.7577 0.6703 0.3250 0.029 Uiso 1 1 d R
H5B H 0.8871 0.7384 0.3446 0.029 Uiso 1 1 d R
H5C H 0.7737 0.7261 0.2511 0.029 Uiso 1 1 d R
N6 N 0.5977(3) 0.7477(3) 0.3925(3) 0.0234(11) Uani 1 1 d .
H6A H 0.5189 0.7479 0.3747 0.035 Uiso 1 1 calc R
H6B H 0.6411 0.7654 0.4661 0.035 Uiso 1 1 calc R
H6C H 0.5900 0.6807 0.3546 0.035 Uiso 1 1 calc R
N7 N -0.1531(3) 0.4129(3) 0.3649(3) 0.0303(13) Uani 1 1 d .
H7A H -0.2314 0.4153 0.3372 0.045 Uiso 1 1 calc R
H7B H -0.1606 0.3483 0.3700 0.045 Uiso 1 1 calc R
H7C H -0.1193 0.4207 0.3194 0.045 Uiso 1 1 calc R
O1W O -0.3350(2) 0.6200(2) 0.0796(2) 0.0277(10) Uani 1 1 d .
O2W O -0.4036(3) 0.3940(3) 0.0260(2) 0.0318(11) Uani 1 1 d .
O11 O 0.6723(3) 0.5263(3) 0.3061(3) 0.0402(12) Uani 1 1 d .
O12 O 0.4757(3) 0.5258(3) 0.2381(3) 0.0393(12) Uani 1 1 d .
O21 O 0.5721(3) 0.3071(3) 0.2205(2) 0.0347(11) Uani 1 1 d .
O22 O 0.3733(2) 0.3030(2) 0.1886(2) 0.0212(9) Uani 1 1 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'
I I -0.4742 1.8119 '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'
O O 0.0106 0.0060 '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
I1 Pb1 I3 96.10(3) . .
I1 Pb1 I4 89.05(3) . .
I3 Pb1 I4 169.748(11) . .
I1 Pb1 I2 91.40(2) . .
I3 Pb1 I2 86.74(2) . .
I4 Pb1 I2 84.269(19) . .
I1 Pb1 I5 171.821(9) . .
I3 Pb1 I5 87.13(3) . .
I4 Pb1 I5 88.96(3) . .
I2 Pb1 I5 96.288(19) . .
I1 Pb1 I6 92.06(2) . .
I3 Pb1 I6 94.77(2) . .
I4 Pb1 I6 93.89(2) . .
I2 Pb1 I6 176.051(8) . .
I5 Pb1 I6 80.163(19) . .
I8 Pb2 I9 92.22(2) . .
I8 Pb2 I7 87.55(2) . .
I9 Pb2 I7 93.13(3) . .
I8 Pb2 I10 84.837(18) . .
I9 Pb2 I10 90.45(3) . .
I7 Pb2 I10 171.707(9) . .
I8 Pb2 I5 97.786(18) . .
I9 Pb2 I5 169.238(9) . .
I7 Pb2 I5 91.26(3) . .
I10 Pb2 I5 86.52(3) . .
I8 Pb2 I2 176.915(7) . 2_576
I9 Pb2 I2 88.49(2) . 2_576
I7 Pb2 I2 89.41(2) . 2_576
I10 Pb2 I2 98.163(18) . 2_576
I5 Pb2 I2 81.731(18) . 2_576
Pb1 I2 Pb2 176.138(9) . 2_576
Pb2 I5 Pb1 176.039(10) . .
Pb2 I10 Pb2 180.0 2_676 .
C2 C1 N1 114.5(4) . .
C2 C1 H1D 108.6 . .
N1 C1 H1D 108.6 . .
C2 C1 H1E 108.6 . .
N1 C1 H1E 108.6 . .
H1D C1 H1E 107.6 . .
C1 C2 N2 113.3(3) . .
C1 C2 H2D 108.9 . .
N2 C2 H2D 108.9 . .
C1 C2 H2E 108.9 . .
N2 C2 H2E 108.9 . .
H2D C2 H2E 107.7 . .
N3 C3 C4 112.3(4) . .
N3 C3 H3D 109.1 . .
C4 C3 H3D 109.1 . .
N3 C3 H3E 109.1 . .
C4 C3 H3E 109.1 . .
H3D C3 H3E 107.9 . .
C3 C4 N4 113.7(3) . .
C3 C4 H4D 108.8 . .
N4 C4 H4D 108.8 . .
C3 C4 H4E 108.8 . .
N4 C4 H4E 108.8 . .
H4D C4 H4E 107.7 . .
N5 C5 C6 113.3(3) . .
N5 C5 H5D 108.9 . .
C6 C5 H5D 108.9 . .
N5 C5 H5E 108.9 . .
C6 C5 H5E 108.9 . .
H5D C5 H5E 107.7 . .
N6 C6 C5 112.1(4) . .
N6 C6 H6D 109.2 . .
C5 C6 H6D 109.2 . .
N6 C6 H6E 109.2 . .
C5 C6 H6E 109.2 . .
H6D C6 H6E 107.9 . .
N7 C7 C7 108.2(4) . 2_566
N7 C7 H7D 110.0 . .
C7 C7 H7D 110.0 2_566 .
N7 C7 H7E 110.0 . .
C7 C7 H7E 110.0 2_566 .
H7D C7 H7E 108.4 . .
O11 C11 O12 122.0(4) . .
O11 C11 C21 120.2(4) . .
O12 C11 C21 117.7(3) . .
O22 C21 O21 127.6(4) . .
O22 C21 C11 119.7(5) . .
O21 C21 C11 112.7(4) . .
C1 N1 H1A 109.5 . .
C1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C1 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C2 N2 H2A 109.5 . .
C2 N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
C2 N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
C3 N3 H3A 109.5 . .
C3 N3 H3B 109.5 . .
H3A N3 H3B 109.5 . .
C3 N3 H3C 109.5 . .
H3A N3 H3C 109.5 . .
H3B N3 H3C 109.5 . .
C4 N4 H4A 109.5 . .
C4 N4 H4B 109.5 . .
H4A N4 H4B 109.5 . .
C4 N4 H4C 109.5 . .
H4A N4 H4C 109.5 . .
H4B N4 H4C 109.5 . .
C5 N5 H5A 112.4 . .
C5 N5 H5B 106.8 . .
H5A N5 H5B 112.2 . .
C5 N5 H5C 106.3 . .
H5A N5 H5C 112.2 . .
H5B N5 H5C 106.6 . .
C6 N6 H6A 109.5 . .
C6 N6 H6B 109.5 . .
H6A N6 H6B 109.5 . .
C6 N6 H6C 109.5 . .
H6A N6 H6C 109.5 . .
H6B N6 H6C 109.5 . .
C7 N7 H7A 109.5 . .
C7 N7 H7B 109.5 . .
H7A N7 H7B 109.5 . .
C7 N7 H7C 109.5 . .
H7A N7 H7C 109.5 . .
H7B N7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.0475(7) .
Pb1 I3 3.1632(8) .
Pb1 I4 3.1691(8) .
Pb1 I2 3.1858(9) .
Pb1 I5 3.3163(8) .
Pb1 I6 3.4621(9) .
Pb2 I8 3.0779(9) .
Pb2 I9 3.0947(7) .
Pb2 I7 3.1037(7) .
Pb2 I10 3.2722(8) .
Pb2 I5 3.2978(8) .
Pb2 I2 3.4021(10) 2_576
I2 Pb2 3.4021(10) 2_576
I10 Pb2 3.2722(8) 2_676
C1 C2 1.444(6) .
C1 N1 1.504(5) .
C1 H1D 0.9700 .
C1 H1E 0.9700 .
C2 N2 1.452(6) .
C2 H2D 0.9700 .
C2 H2E 0.9700 .
C3 N3 1.435(7) .
C3 C4 1.487(6) .
C3 H3D 0.9700 .
C3 H3E 0.9700 .
C4 N4 1.490(6) .
C4 H4D 0.9700 .
C4 H4E 0.9700 .
C5 N5 1.481(6) .
C5 C6 1.523(6) .
C5 H5D 0.9700 .
C5 H5E 0.9700 .
C6 N6 1.489(6) .
C6 H6D 0.9700 .
C6 H6E 0.9700 .
C7 N7 1.470(4) .
C7 C7 1.545(8) 2_566
C7 H7D 0.9700 .
C7 H7E 0.9700 .
C11 O11 1.239(4) .
C11 O12 1.276(6) .
C11 C21 1.529(6) .
C21 O22 1.255(5) .
C21 O21 1.258(7) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N3 H3C 0.8900 .
N4 H4A 0.8900 .
N4 H4B 0.8900 .
N4 H4C 0.8900 .
N5 H5A 0.8901 .
N5 H5B 0.8900 .
N5 H5C 0.8899 .
N6 H6A 0.8900 .
N6 H6B 0.8900 .
N6 H6C 0.8900 .
N7 H7A 0.8900 .
N7 H7B 0.8900 .
N7 H7C 0.8900 .
