#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:46:30 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188149 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/06/7040655.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_7040655
loop_
_publ_author_name
'Romero, María J'
'Carballido, Rocío'
'Rodríguez-Silva, Laura'
'Maneiro, Marcelino'
'Zaragoza, Guillermo'
'González-Noya, Ana M'
'Pedrido, Rosa'
_publ_section_title
;
 An unusual assembled Pb(ii) meso-helicate that shows the inert pair
 effect.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16162
_journal_page_last               16165
_journal_paper_doi               10.1039/c6dt03106d
_journal_volume                  45
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H20 N4 O4 Pb1'
_chemical_formula_sum            'C24 H20 N4 O4 Pb'
_chemical_formula_weight         635.63
_chemical_name_common            '[Pb2(L)2] '
_chemical_name_systematic        2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-05-19T13:51:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-06-22 deposited with the CCDC.
2016-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.584(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4274(4)
_cell_length_b                   10.6731(3)
_cell_length_c                   17.2083(5)
_cell_measurement_reflns_used    1979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.29
_cell_measurement_wavelength     0.71073
_cell_volume                     2136.77(11)
_computing_cell_refinement       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_collection       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX2 (BRUKER AXS, 2005)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-08  (Beurskens et all, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25486
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    7.937
_exptl_absorpt_correction_T_max  0.451
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_recrystallization_method
'Recrystallization from the mother liquors '
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4708
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0333
_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)+(0.0252P)²+3.6669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                3603
_reflns_number_total             4708
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c6dt03106d2.cif
_cod_data_source_block           L1-Pb
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_monochromador' tag replaced with
'_diffrn_radiation_monochromator' tag as specified in the replacement
file
'/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/lists/replacement-tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7040655.cif.
;
_cod_database_code               7040655
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.5305(4) 0.1472(5) -0.1378(3) 0.0214(12) Uani 1 1 d .
C2 C 0.5928(5) 0.1154(6) -0.1892(4) 0.0298(14) Uani 1 1 d .
H2 H 0.6366 0.176 -0.2032 0.036 Uiso 1 1 calc R
C3 C 0.5894(5) -0.0045(5) -0.2187(3) 0.0291(15) Uani 1 1 d .
H3 H 0.6304 -0.0242 -0.253 0.035 Uiso 1 1 calc R
C4 C 0.5260(5) -0.0962(6) -0.1981(3) 0.0249(12) Uani 1 1 d .
H4 H 0.5268 -0.1779 -0.2166 0.03 Uiso 1 1 calc R
C5 C 0.4615(5) -0.0663(5) -0.1500(3) 0.0218(12) Uani 1 1 d .
H5 H 0.417 -0.1278 -0.1377 0.026 Uiso 1 1 calc R
C6 C 0.4618(4) 0.0552(5) -0.1195(3) 0.0218(12) Uani 1 1 d .
C7 C 0.3875(4) 0.0861(5) -0.0708(3) 0.0207(12) Uani 1 1 d .
C8 C 0.4360(4) 0.4092(5) 0.0613(3) 0.0240(12) Uani 1 1 d .
H8A H 0.4987 0.3782 0.1079 0.036 Uiso 1 1 calc R
H8B H 0.4157 0.4919 0.0734 0.036 Uiso 1 1 calc R
H8C H 0.4585 0.4122 0.0134 0.036 Uiso 1 1 calc R
C9 C 0.3349(4) 0.3243(5) 0.0444(3) 0.0183(11) Uani 1 1 d .
C10 C 0.2482(4) 0.3508(5) 0.0823(3) 0.0169(11) Uani 1 1 d .
C11 C 0.2752(5) 0.4097(5) 0.1591(3) 0.0229(12) Uani 1 1 d .
H11 H 0.3493 0.4392 0.1864 0.028 Uiso 1 1 calc R
C12 C 0.1917(5) 0.4244(5) 0.1949(3) 0.0243(12) Uani 1 1 d .
H12 H 0.2106 0.464 0.2461 0.029 Uiso 1 1 calc R
C13 C 0.0807(5) 0.3809(5) 0.1552(3) 0.0228(12) Uani 1 1 d .
H13 H 0.0254 0.3913 0.1796 0.027 Uiso 1 1 calc R
C14 C 0.0526(4) 0.3216(5) 0.0786(3) 0.0197(12) Uani 1 1 d .
C15 C 0.1345(4) 0.3119(5) 0.0410(3) 0.0173(11) Uani 1 1 d .
H15 H 0.1137 0.2791 -0.0124 0.021 Uiso 1 1 calc R
C16 C -0.1506(5) 0.3210(5) -0.0310(3) 0.0256(13) Uani 1 1 d .
H16A H -0.2173 0.2682 -0.051 0.038 Uiso 1 1 calc R
H16B H -0.1228 0.338 -0.0754 0.038 Uiso 1 1 calc R
H16C H -0.1706 0.3983 -0.011 0.038 Uiso 1 1 calc R
C17 C -0.0604(4) 0.2571(5) 0.0370(3) 0.0208(12) Uani 1 1 d .
C18 C 0.0051(4) -0.0243(6) 0.1382(3) 0.0205(11) Uani 1 1 d .
C19 C 0.0923(4) -0.0780(5) 0.2140(3) 0.0205(12) Uani 1 1 d .
C20 C 0.1669(5) -0.0004(5) 0.2770(3) 0.0242(13) Uani 1 1 d .
C21 C 0.2401(5) -0.0541(6) 0.3494(3) 0.0316(15) Uani 1 1 d .
H21 H 0.2868 -0.0032 0.3917 0.038 Uiso 1 1 calc R
C22 C 0.2445(5) -0.1823(6) 0.3594(4) 0.0320(15) Uani 1 1 d .
H22 H 0.2958 -0.2176 0.4076 0.038 Uiso 1 1 calc R
C23 C 0.1732(5) -0.2584(6) 0.2981(3) 0.0283(14) Uani 1 1 d .
H23 H 0.1763 -0.3449 0.305 0.034 Uiso 1 1 calc R
C24 C 0.0981(5) -0.2069(6) 0.2274(3) 0.0245(13) Uani 1 1 d .
H24 H 0.0494 -0.2592 0.1869 0.029 Uiso 1 1 calc R
N1 N 0.3970(4) 0.1999(4) -0.0402(3) 0.0200(10) Uani 1 1 d .
N2 N 0.3197(4) 0.2236(4) 0.0004(3) 0.0187(10) Uani 1 1 d .
N3 N -0.0763(4) 0.1448(4) 0.0585(3) 0.0212(10) Uani 1 1 d .
N4 N 0.0144(4) 0.0963(5) 0.1265(3) 0.0237(10) Uani 1 1 d D
O1 O 0.5383(3) 0.2641(4) -0.1100(3) 0.0310(10) Uani 1 1 d .
H1 H 0.4951 0.2735 -0.0838 0.047 Uiso 1 1 calc R
O2 O 0.3188(3) -0.0037(3) -0.0629(2) 0.0257(9) Uani 1 1 d .
O3 O -0.0709(3) -0.0988(3) 0.0915(2) 0.0255(9) Uani 1 1 d .
O4 O 0.1709(4) 0.1257(4) 0.2711(3) 0.0353(10) Uani 1 1 d D
H4A H 0.132(4) 0.141(5) 0.2224(17) 0.053 Uiso 1 1 d D
Pb1 Pb 0.216760(17) 0.03002(2) 0.021099(12) 0.01940(7) 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 0 '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 0.006 '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
O1 C1 C2 117.8(5) . .
O1 C1 C6 123.3(5) . .
C2 C1 C6 118.9(5) . .
C3 C2 C1 120.4(6) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
C2 C3 C4 120.9(5) . .
C2 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
C5 C4 C3 119.7(5) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C4 C5 C6 121.0(5) . .
C4 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
C5 C6 C1 119.0(5) . .
C5 C6 C7 119.8(5) . .
C1 C6 C7 121.2(5) . .
N1 C7 O2 126.8(5) . .
N1 C7 C6 116.5(5) . .
O2 C7 C6 116.7(5) . .
C9 C8 H8A 109.5 . .
C9 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C9 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N2 C9 C10 116.2(5) . .
N2 C9 C8 124.1(5) . .
C10 C9 C8 119.7(5) . .
C11 C10 C15 118.5(5) . .
C11 C10 C9 122.6(5) . .
C15 C10 C9 118.9(4) . .
C12 C11 C10 120.3(5) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C13 C12 C11 120.8(5) . .
C13 C12 H12 119.6 . .
C11 C12 H12 119.6 . .
C12 C13 C14 119.6(5) . .
C12 C13 H13 120.2 . .
C14 C13 H13 120.2 . .
C15 C14 C13 119.6(5) . .
C15 C14 C17 117.3(5) . .
C13 C14 C17 122.9(5) . .
C14 C15 C10 120.9(5) . .
C14 C15 H15 119.5 . .
C10 C15 H15 119.5 . .
C17 C16 H16A 109.5 . .
C17 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C17 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N3 C17 C16 120.5(5) . .
N3 C17 C14 120.1(5) . .
C16 C17 C14 119.4(5) . .
O3 C18 N4 126.7(5) . .
O3 C18 C19 117.4(5) . .
N4 C18 C19 115.8(5) . .
C24 C19 C20 118.0(5) . .
C24 C19 C18 120.3(5) . .
C20 C19 C18 121.6(5) . .
O4 C20 C21 116.7(5) . .
O4 C20 C19 123.8(5) . .
C21 C20 C19 119.5(5) . .
C22 C21 C20 120.6(6) . .
C22 C21 H21 119.7 . .
C20 C21 H21 119.7 . .
C21 C22 C23 120.2(5) . .
C21 C22 H22 119.9 . .
C23 C22 H22 119.9 . .
C24 C23 C22 120.0(6) . .
C24 C23 H23 120 . .
C22 C23 H23 120 . .
C23 C24 C19 121.7(5) . .
C23 C24 H24 119.2 . .
C19 C24 H24 119.2 . .
C7 N1 N2 112.9(4) . .
C9 N2 N1 117.4(4) . .
C9 N2 Pb1 125.3(3) . .
N1 N2 Pb1 113.3(3) . .
C17 N3 N4 114.9(4) . .
C17 N3 Pb1 131.3(4) . 3
N4 N3 Pb1 111.6(3) . 3
C18 N4 N3 113.6(4) . .
C1 O1 H1 109.5 . .
C7 O2 Pb1 118.6(3) . .
C18 O3 Pb1 121.9(4) . 3
C20 O4 H4A 104(4) . .
O3 Pb1 O2 87.96(14) 3 .
O3 Pb1 N2 84.62(13) 3 .
O2 Pb1 N2 67.27(13) . .
O3 Pb1 N3 65.98(13) 3 3
O2 Pb1 N3 88.44(13) . 3
N2 Pb1 N3 142.77(13) . 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.327(6) .
C1 C2 1.406(8) .
C1 C6 1.407(7) .
C2 C3 1.372(8) .
C2 H2 0.93 .
C3 C4 1.378(8) .
C3 H3 0.93 .
C4 C5 1.377(7) .
C4 H4 0.93 .
C5 C6 1.399(7) .
C5 H5 0.93 .
C6 C7 1.486(7) .
C7 N1 1.312(7) .
C7 O2 1.322(6) .
C8 C9 1.492(7) .
C8 H8A 0.96 .
C8 H8B 0.96 .
C8 H8C 0.96 .
C9 N2 1.290(6) .
C9 C10 1.470(7) .
C10 C11 1.393(7) .
C10 C15 1.403(7) .
C11 C12 1.389(7) .
C11 H11 0.93 .
C12 C13 1.387(7) .
C12 H12 0.93 .
C13 C14 1.391(7) .
C13 H13 0.93 .
C14 C15 1.390(7) .
C14 C17 1.500(7) .
C15 H15 0.93 .
C16 C17 1.473(7) .
C16 H16A 0.96 .
C16 H16B 0.96 .
C16 H16C 0.96 .
C17 N3 1.290(7) .
C18 O3 1.279(6) .
C18 N4 1.314(7) .
C18 C19 1.488(7) .
C19 C24 1.392(8) .
C19 C20 1.419(7) .
C20 O4 1.351(6) .
C20 C21 1.383(8) .
C21 C22 1.378(8) .
C21 H21 0.93 .
C22 C23 1.379(8) .
C22 H22 0.93 .
C23 C24 1.362(7) .
C23 H23 0.93 .
C24 H24 0.93 .
N1 N2 1.396(6) .
N2 Pb1 2.520(4) .
N3 N4 1.407(6) .
N3 Pb1 2.593(4) 3
O1 H1 0.82 .
O2 Pb1 2.261(4) .
O3 Pb1 2.260(4) 3
O4 H4A 0.825(18) .
Pb1 O3 2.260(4) 3
Pb1 N3 2.593(4) 3
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_4
O1 C1 C2 C3 179.0(5) . .
C6 C1 C2 C3 -2.0(8) . .
C1 C2 C3 C4 -0.6(9) . .
C2 C3 C4 C5 2.6(9) . .
C3 C4 C5 C6 -1.9(8) . .
C4 C5 C6 C1 -0.7(8) . .
C4 C5 C6 C7 177.4(5) . .
O1 C1 C6 C5 -178.4(5) . .
C2 C1 C6 C5 2.6(8) . .
O1 C1 C6 C7 3.5(8) . .
C2 C1 C6 C7 -175.4(5) . .
C5 C6 C7 N1 176.3(5) . .
C1 C6 C7 N1 -5.7(7) . .
C5 C6 C7 O2 -3.7(7) . .
C1 C6 C7 O2 174.4(5) . .
N2 C9 C10 C11 146.7(5) . .
C8 C9 C10 C11 -30.6(7) . .
N2 C9 C10 C15 -31.3(7) . .
C8 C9 C10 C15 151.4(5) . .
C15 C10 C11 C12 2.6(8) . .
C9 C10 C11 C12 -175.3(5) . .
C10 C11 C12 C13 0.1(9) . .
C11 C12 C13 C14 0.1(8) . .
C12 C13 C14 C15 -3.0(8) . .
C12 C13 C14 C17 171.7(5) . .
C13 C14 C15 C10 5.8(8) . .
C17 C14 C15 C10 -169.2(5) . .
C11 C10 C15 C14 -5.6(8) . .
C9 C10 C15 C14 172.4(5) . .
C15 C14 C17 N3 93.4(6) . .
C13 C14 C17 N3 -81.5(7) . .
C15 C14 C17 C16 -83.9(6) . .
C13 C14 C17 C16 101.3(6) . .
O3 C18 C19 C24 7.6(7) . .
N4 C18 C19 C24 -172.7(5) . .
O3 C18 C19 C20 -168.5(5) . .
N4 C18 C19 C20 11.2(7) . .
C24 C19 C20 O4 179.0(5) . .
C18 C19 C20 O4 -4.8(8) . .
C24 C19 C20 C21 -1.4(7) . .
C18 C19 C20 C21 174.8(5) . .
O4 C20 C21 C22 -177.7(5) . .
C19 C20 C21 C22 2.7(8) . .
C20 C21 C22 C23 -2.0(8) . .
C21 C22 C23 C24 0.1(8) . .
C22 C23 C24 C19 1.2(8) . .
C20 C19 C24 C23 -0.5(8) . .
C18 C19 C24 C23 -176.7(5) . .
O2 C7 N1 N2 -3.6(7) . .
C6 C7 N1 N2 176.5(4) . .
C10 C9 N2 N1 176.4(4) . .
C8 C9 N2 N1 -6.4(7) . .
C10 C9 N2 Pb1 -27.9(6) . .
C8 C9 N2 Pb1 149.2(4) . .
C7 N1 N2 C9 168.6(5) . .
C7 N1 N2 Pb1 10.1(5) . .
C16 C17 N3 N4 -177.4(4) . .
C14 C17 N3 N4 5.3(7) . .
C16 C17 N3 Pb1 21.0(7) . 3
C14 C17 N3 Pb1 -156.2(4) . 3
O3 C18 N4 N3 5.5(8) . .
C19 C18 N4 N3 -174.2(4) . .
C17 N3 N4 C18 -169.1(5) . .
Pb1 N3 N4 C18 -3.9(5) 3 .
N1 C7 O2 Pb1 -6.1(7) . .
C6 C7 O2 Pb1 173.8(3) . .
N4 C18 O3 Pb1 -4.0(7) . 3
C19 C18 O3 Pb1 175.7(3) . 3
C7 O2 Pb1 O3 92.9(4) . 3
C7 O2 Pb1 N2 7.9(3) . .
C7 O2 Pb1 N3 159.0(4) . 3
C9 N2 Pb1 O3 103.9(4) . 3
N1 N2 Pb1 O3 -99.6(3) . 3
C9 N2 Pb1 O2 -166.1(5) . .
N1 N2 Pb1 O2 -9.5(3) . .
C9 N2 Pb1 N3 140.8(4) . 3
N1 N2 Pb1 N3 -62.7(4) . 3
