#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/07/7050727.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_7050727
loop_
_publ_author_name
'Arya, Pious'
'Channa, Asif'
'Cragg, Peter J.'
'Prince, Paul D.'
'Steed, Jonathan W.'
_publ_section_title
;
 C-Donor lariat ether 'scorpionates'
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              440
_journal_paper_doi               10.1039/b108522k
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C13 H25 N3 O10 Pb'
_chemical_formula_weight         590.55
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.365(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2947(2)
_cell_length_b                   13.6796(6)
_cell_length_c                   15.3903(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1944.78(11)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11648
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.59
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.731
_exptl_absorpt_correction_T_max  0.6693
_exptl_absorpt_correction_T_min  0.2741
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.983
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.00191(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0162P)²+1.8293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                3981
_reflns_number_total             4437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108522k.txt
_cod_data_source_block           pbnoal15
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7050727
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Pb1 Pb 0.922744(12) 0.821368(10) 0.190378(8) 0.01365(7) Uani 1 1 d . A .
O1 O 0.7821(2) 0.8896(2) 0.31656(16) 0.0189(5) Uani 1 1 d . . .
N1 N 1.0710(3) 0.9536(3) 0.2951(2) 0.0182(7) Uani 1 1 d . . .
C1 C 1.3409(4) 0.9064(4) 0.4789(3) 0.0324(10) Uani 1 1 d . . .
H1A H 1.3078 0.8429 0.4919 0.039 Uiso 1 1 calc R . .
H1B H 1.4041 0.9409 0.5210 0.039 Uiso 1 1 calc R . .
O2 O 0.6396(3) 0.7664(2) 0.19280(18) 0.0204(6) Uani 1 1 d . . .
N2 N 0.9833(3) 0.6213(2) 0.2791(2) 0.0210(7) Uani 1 1 d . A 1
C2 C 1.2993(4) 0.9465(3) 0.4028(3) 0.0286(10) Uani 1 1 d . . .
H2 H 1.3336 1.0100 0.3910 0.034 Uiso 1 1 calc R . .
O3 O 0.7321(3) 0.8600(2) 0.04491(18) 0.0207(6) Uani 1 1 d . . .
N3 N 1.1567(3) 0.7448(3) 0.0849(2) 0.0203(7) Uani 1 1 d . A 1
C3 C 1.2001(4) 0.8959(3) 0.3338(3) 0.0251(9) Uani 1 1 d . . .
H3A H 1.1649 0.8351 0.3593 0.030 Uiso 1 1 calc R . .
H3B H 1.2571 0.8767 0.2859 0.030 Uiso 1 1 calc R . .
O4 O 0.9327(3) 0.9998(2) 0.12253(17) 0.0203(6) Uani 1 1 d . . .
C4 C 0.9835(4) 0.9892(3) 0.3644(2) 0.0198(8) Uani 1 1 d . . .
H4A H 0.9271 1.0472 0.3423 0.024 Uiso 1 1 calc R . .
H4B H 1.0497 1.0098 0.4160 0.024 Uiso 1 1 calc R . .
O5 O 0.9742(3) 0.7009(2) 0.32026(19) 0.0255(6) Uani 1 1 d . . .
C5 C 0.8811(4) 0.9127(3) 0.3922(2) 0.0199(8) Uani 1 1 d . . .
H5A H 0.9354 0.8536 0.4136 0.024 Uiso 1 1 calc R . .
H5B H 0.8279 0.9382 0.4396 0.024 Uiso 1 1 calc R . .
O6 O 0.9467(3) 0.6213(2) 0.19773(18) 0.0346(8) Uani 1 1 d . . .
C6 C 0.6620(4) 0.8301(3) 0.3365(3) 0.0221(9) Uani 1 1 d . . .
H6A H 0.6109 0.8619 0.3820 0.027 Uiso 1 1 calc R . .
H6B H 0.6969 0.7653 0.3584 0.027 Uiso 1 1 calc R . .
O7 O 1.0270(3) 0.5465(2) 0.31751(19) 0.0307(7) Uani 1 1 d . A 1
C7 C 0.5626(4) 0.8188(3) 0.2541(3) 0.0227(9) Uani 1 1 d . . .
H7A H 0.4748 0.7822 0.2657 0.027 Uiso 1 1 calc R . .
H7B H 0.5326 0.8838 0.2303 0.027 Uiso 1 1 calc R . .
O8 O 1.1865(3) 0.7678(3) 0.16417(19) 0.0334(8) Uani 1 1 d . . .
C8 C 0.5623(4) 0.7614(3) 0.1064(3) 0.0260(9) Uani 1 1 d . . .
H8A H 0.4582 0.7510 0.1114 0.031 Uiso 1 1 calc R . .
H8B H 0.5978 0.7046 0.0751 0.031 Uiso 1 1 calc R . .
O9 O 1.0436(3) 0.7794(2) 0.04310(19) 0.0261(6) Uani 1 1 d . . .
C9 C 0.5800(4) 0.8524(3) 0.0538(3) 0.0227(9) Uani 1 1 d . . .
H9A H 0.5231 0.8474 -0.0043 0.027 Uiso 1 1 calc R . .
H9B H 0.5466 0.9105 0.0843 0.027 Uiso 1 1 calc R . .
O10 O 1.2341(3) 0.6869(2) 0.0496(2) 0.0357(8) Uani 1 1 d . A 1
C10 C 0.7709(4) 0.9474(3) 0.0020(3) 0.0276(9) Uani 1 1 d . . .
H10A H 0.6893 0.9673 -0.0412 0.033 Uiso 1 1 calc R . .
H10B H 0.8551 0.9336 -0.0302 0.033 Uiso 1 1 calc R . .
C11 C 0.8079(4) 1.0300(3) 0.0643(3) 0.0264(9) Uani 1 1 d . . .
H11A H 0.8304 1.0896 0.0320 0.032 Uiso 1 1 calc R . .
H11B H 0.7254 1.0442 0.0979 0.032 Uiso 1 1 calc R . .
C12 C 0.9879(4) 1.0762(3) 0.1808(3) 0.0245(9) Uani 1 1 d . . .
H12A H 0.9110 1.0998 0.2151 0.029 Uiso 1 1 calc R . .
H12B H 1.0211 1.1318 0.1470 0.029 Uiso 1 1 calc R . .
C13 C 1.1131(4) 1.0357(3) 0.2413(3) 0.0229(8) Uani 1 1 d . . .
H13A H 1.1897 1.0135 0.2060 0.027 Uiso 1 1 calc R . .
H13B H 1.1542 1.0886 0.2804 0.027 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'
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'
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
_geom_angle_publ_flag
O5 Pb1 O1 73.78(9) . . ?
O5 Pb1 O8 81.13(10) . . ?
O1 Pb1 O8 139.45(8) . . ?
O5 Pb1 O4 150.92(8) . . ?
O1 Pb1 O4 90.35(8) . . ?
O8 Pb1 O4 97.01(10) . . ?
O5 Pb1 N1 85.83(10) . . ?
O1 Pb1 N1 65.40(8) . . ?
O8 Pb1 N1 81.70(9) . . ?
O4 Pb1 N1 65.28(9) . . ?
O5 Pb1 O9 116.95(9) . . ?
O1 Pb1 O9 169.24(8) . . ?
O8 Pb1 O9 48.01(8) . . ?
O4 Pb1 O9 80.21(9) . . ?
N1 Pb1 O9 114.30(9) . . ?
O5 Pb1 O2 84.85(9) . . ?
O1 Pb1 O2 62.01(8) . . ?
O8 Pb1 O2 146.86(10) . . ?
O4 Pb1 O2 109.41(8) . . ?
N1 Pb1 O2 127.12(8) . . ?
O9 Pb1 O2 116.26(8) . . ?
O5 Pb1 O6 47.78(9) . . ?
O1 Pb1 O6 111.57(9) . . ?
O8 Pb1 O6 69.89(11) . . ?
O4 Pb1 O6 157.52(8) . . ?
N1 Pb1 O6 127.56(9) . . ?
O9 Pb1 O6 77.49(9) . . ?
O2 Pb1 O6 78.43(9) . . ?
O5 Pb1 O3 142.86(9) . . ?
O1 Pb1 O3 101.82(8) . . ?
O8 Pb1 O3 117.13(8) . . ?
O4 Pb1 O3 63.32(8) . . ?
N1 Pb1 O3 126.75(9) . . ?
O9 Pb1 O3 69.39(8) . . ?
O2 Pb1 O3 62.01(8) . . ?
O6 Pb1 O3 105.50(9) . . ?
C5 O1 C6 113.2(3) . . ?
C5 O1 Pb1 110.47(19) . . ?
C6 O1 Pb1 114.6(2) . . ?
C13 N1 C4 110.6(3) . . ?
C13 N1 C3 111.9(3) . . ?
C4 N1 C3 111.2(3) . . ?
C13 N1 Pb1 109.0(2) . . ?
C4 N1 Pb1 111.3(2) . . ?
C3 N1 Pb1 102.6(2) . . ?
C7 O2 C8 113.3(3) . . ?
C7 O2 Pb1 114.9(2) . . ?
C8 O2 Pb1 112.4(2) . . ?
O7 N2 O6 121.2(3) . . ?
O7 N2 O5 120.8(3) . . ?
O6 N2 O5 118.1(3) . . ?
C1 C2 C3 122.5(4) . . ?
C10 O3 C9 113.9(3) . . ?
C10 O3 Pb1 111.4(2) . . ?
C9 O3 Pb1 117.4(2) . . ?
O10 N3 O8 120.6(3) . . ?
O10 N3 O9 120.6(3) . . ?
O8 N3 O9 118.8(3) . . ?
C2 C3 N1 116.2(4) . . ?
C12 O4 C11 112.8(3) . . ?
C12 O4 Pb1 116.7(2) . . ?
C11 O4 Pb1 116.4(2) . . ?
N1 C4 C5 112.8(3) . . ?
N2 O5 Pb1 100.2(2) . . ?
O1 C5 C4 106.9(3) . . ?
N2 O6 Pb1 93.1(2) . . ?
O1 C6 C7 107.4(3) . . ?
O2 C7 C6 107.6(3) . . ?
N3 O8 Pb1 96.3(2) . . ?
O2 C8 C9 112.6(3) . . ?
N3 O9 Pb1 93.0(2) . . ?
O3 C9 C8 106.2(3) . . ?
O3 C10 C11 112.7(3) . . ?
O4 C11 C10 107.1(3) . . ?
O4 C12 C13 108.4(3) . . ?
N1 C13 C12 113.0(3) . . ?
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
Pb1 O5 2.594(3) . ?
Pb1 O1 2.630(2) . ?
Pb1 O8 2.632(3) . ?
Pb1 O4 2.661(3) . ?
Pb1 N1 2.697(3) . ?
Pb1 O9 2.701(3) . ?
Pb1 O2 2.742(2) . ?
Pb1 O6 2.747(3) . ?
Pb1 O3 2.748(3) . ?
O1 C5 1.437(4) . ?
O1 C6 1.441(4) . ?
N1 C13 1.474(5) . ?
N1 C4 1.492(5) . ?
N1 C3 1.503(5) . ?
C1 C2 1.312(6) . ?
O2 C7 1.438(5) . ?
O2 C8 1.441(5) . ?
N2 O7 1.229(4) . ?
N2 O6 1.260(4) . ?
N2 O5 1.267(4) . ?
C2 C3 1.496(5) . ?
O3 C10 1.431(5) . ?
O3 C9 1.440(4) . ?
N3 O10 1.235(4) . ?
N3 O8 1.261(4) . ?
N3 O9 1.261(4) . ?
O4 C12 1.434(5) . ?
O4 C11 1.445(4) . ?
C4 C5 1.507(5) . ?
C6 C7 1.492(6) . ?
C8 C9 1.503(6) . ?
C10 C11 1.497(6) . ?
C12 C13 1.513(6) . ?
