#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/90/7019040.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_7019040
loop_
_publ_author_name
'Jin, Juan'
'Bai, Fu-Quan'
'Jia, Ming-Jun'
'Yu, Jie-Hui'
'Xu, Ji-Qing'
_publ_section_title
;
 New monoacylhydrazidate-coordinated Mn2+ and Pb2+ compounds
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              6137
_journal_paper_doi               10.1039/c2dt30389b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C16 H12.5 N6 O4.25 Pb'
_chemical_formula_weight         564.01
_chemical_name_systematic
;
?
;
_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                 94.977(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.0000(3)
_cell_length_b                   31.157(3)
_cell_length_c                   12.9587(12)
_cell_measurement_temperature    293(2)
_cell_volume                     1608.9(2)
_computing_cell_refinement       'Bruker SMAR'
_computing_data_collection       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Siements SMART CCD'
_diffrn_measurement_method       'Omega scan'
_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  0.1059
_diffrn_reflns_av_sigmaI/netI    0.1505
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11663
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    10.528
_exptl_absorpt_correction_T_max  0.349
_exptl_absorpt_correction_T_min  0.336
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.042
_refine_diff_density_min         -2.364
_refine_diff_density_rms         0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.0638
_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)+(0.0750P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1814
_reflns_number_gt                1775
_reflns_number_total             4013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30389b.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C16 H12.50 N6 O4.25 Pb'
_cod_database_code               7019040
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
Pb1 Pb 0.59116(14) 0.18593(2) 0.56406(5) 0.0536(3) Uani 1 1 d .
O1 O 0.198(3) 0.1534(3) 0.6650(8) 0.052(3) Uani 1 1 d .
O2 O 0.305(3) -0.0162(3) 0.6059(9) 0.062(3) Uani 1 1 d .
O3 O 0.175(3) 0.1764(3) 0.4144(8) 0.059(3) Uani 1 1 d .
O4 O -0.267(3) 0.2522(4) 0.0608(10) 0.077(4) Uani 1 1 d .
OW1 O 0.145(10) 0.2233(15) 0.909(4) 0.086(19) Uani 0.25 1 d P
N1 N 0.360(3) 0.0966(4) 0.5740(9) 0.041(3) Uani 1 1 d .
N2 N 0.383(3) 0.0525(4) 0.5644(9) 0.047(3) Uani 1 1 d .
H2A H 0.4853 0.0430 0.5133 0.057 Uiso 1 1 calc R
N3 N -0.055(5) 0.1370(8) 0.8453(15) 0.121(8) Uani 1 1 d .
H3A H 0.0191 0.1556 0.8039 0.146 Uiso 1 1 calc R
H3B H -0.1389 0.1453 0.9008 0.146 Uiso 1 1 calc R
N4 N 0.135(3) 0.2320(5) 0.3061(11) 0.067(4) Uani 1 1 d .
H4A H 0.2733 0.2451 0.3498 0.080 Uiso 1 1 calc R
N5 N 0.014(3) 0.2540(4) 0.2151(13) 0.071(5) Uani 1 1 d .
N6 N -0.119(3) 0.1031(4) 0.3595(11) 0.063(4) Uani 1 1 d .
H6A H -0.1706 0.0768 0.3702 0.076 Uiso 1 1 calc R
H6B H 0.0119 0.1167 0.4046 0.076 Uiso 1 1 calc R
C1 C -0.040(5) 0.0950(6) 0.823(2) 0.088(8) Uani 1 1 d .
C2 C -0.170(4) 0.0630(8) 0.8883(13) 0.068(5) Uani 1 1 d .
H2B H -0.2809 0.0717 0.9449 0.082 Uiso 1 1 calc R
C3 C -0.137(5) 0.0222(7) 0.8707(17) 0.077(6) Uani 1 1 d .
H3C H -0.2136 0.0026 0.9172 0.093 Uiso 1 1 calc R
C4 C 0.004(4) 0.0077(6) 0.7871(14) 0.062(5) Uani 1 1 d .
H4B H 0.0266 -0.0215 0.7757 0.075 Uiso 1 1 calc R
C5 C 0.116(3) 0.0381(5) 0.7167(12) 0.043(4) Uani 1 1 d .
C6 C 0.099(4) 0.0833(5) 0.7318(12) 0.043(4) Uani 1 1 d .
C7 C 0.228(4) 0.1107(5) 0.6544(12) 0.042(4) Uani 1 1 d .
C8 C 0.261(4) 0.0228(5) 0.6275(13) 0.048(4) Uani 1 1 d .
C9 C -0.245(4) 0.1236(5) 0.2700(12) 0.044(4) Uani 1 1 d .
C10 C -0.460(4) 0.1022(6) 0.1943(15) 0.064(5) Uani 1 1 d .
H10A H -0.5224 0.0738 0.2038 0.077 Uiso 1 1 calc R
C11 C -0.573(4) 0.1239(5) 0.1081(14) 0.053(4) Uani 1 1 d .
H11A H -0.7211 0.1101 0.0595 0.063 Uiso 1 1 calc R
C12 C -0.480(4) 0.1656(6) 0.0887(13) 0.062(5) Uani 1 1 d .
H12A H -0.5549 0.1786 0.0264 0.074 Uiso 1 1 calc R
C13 C -0.274(3) 0.1884(5) 0.1621(12) 0.044(4) Uani 1 1 d .
C14 C -0.150(4) 0.1667(5) 0.2544(12) 0.041(3) Uani 1 1 d .
C15 C 0.047(3) 0.1916(5) 0.3280(12) 0.042(4) Uani 1 1 d .
C16 C -0.178(4) 0.2318(6) 0.1459(16) 0.065(5) 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'
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
O1 Pb1 O4 85.9(4) . 4_666
O1 Pb1 O3 86.9(4) . .
O4 Pb1 O3 73.8(4) 4_666 .
O1 Pb1 N5 77.1(4) . 4_666
O4 Pb1 N5 50.3(4) 4_666 4_666
O3 Pb1 N5 122.3(4) . 4_666
C7 O1 Pb1 107.3(9) . .
C15 O3 Pb1 146.7(10) . .
C16 O4 Pb1 105.0(10) . 4_565
C7 N1 N2 116.5(12) . .
C8 N2 N1 126.5(13) . .
C15 N4 N5 123.7(12) . .
C16 N5 N4 116.6(13) . .
C16 N5 Pb1 88.1(11) . 4_565
N4 N5 Pb1 151.0(10) . 4_565
N3 C1 C6 118(2) . .
N3 C1 C2 122(3) . .
C6 C1 C2 120.6(17) . .
C3 C2 C1 122(2) . .
C2 C3 C4 122(2) . .
C3 C4 C5 118.3(19) . .
C4 C5 C8 118.3(16) . .
C4 C5 C6 123.5(16) . .
C8 C5 C6 118.2(14) . .
C1 C6 C5 113.6(15) . .
C1 C6 C7 128.7(17) . .
C5 C6 C7 117.6(14) . .
N1 C7 O1 118.0(14) . .
N1 C7 C6 123.8(14) . .
O1 C7 C6 118.1(14) . .
O2 C8 N2 117.3(15) . .
O2 C8 C5 125.4(15) . .
N2 C8 C5 117.1(14) . .
N6 C9 C10 121.4(15) . .
N6 C9 C14 118.4(14) . .
C10 C9 C14 120.2(15) . .
C11 C10 C9 118.6(17) . .
C10 C11 C12 123.0(16) . .
C11 C12 C13 120.5(16) . .
C12 C13 C14 118.1(15) . .
C12 C13 C16 122.2(15) . .
C14 C13 C16 119.7(14) . .
C9 C14 C15 124.4(14) . .
C9 C14 C13 119.5(14) . .
C15 C14 C13 116.0(13) . .
O3 C15 N4 116.0(14) . .
O3 C15 C14 122.9(14) . .
N4 C15 C14 120.8(13) . .
O4 C16 N5 114.9(15) . .
O4 C16 C13 122.2(17) . .
N5 C16 C13 122.9(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.362(11) .
Pb1 O4 2.400(12) 4_666
Pb1 O3 2.463(11) .
Pb1 N5 2.744(14) 4_666
O1 C7 1.342(16) .
O2 C8 1.263(18) .
O3 C15 1.280(17) .
O4 C16 1.30(2) .
O4 Pb1 2.400(12) 4_565
N1 C7 1.286(18) .
N1 N2 1.384(16) .
N2 C8 1.353(19) .
N3 C1 1.34(3) .
N4 C15 1.343(19) .
N4 N5 1.414(18) .
N5 C16 1.32(2) .
N5 Pb1 2.744(14) 4_565
N6 C9 1.381(19) .
C1 C6 1.40(3) .
C1 C2 1.43(3) .
C2 C3 1.30(3) .
C3 C4 1.34(2) .
C4 C5 1.42(2) .
C5 C8 1.42(2) .
C5 C6 1.42(2) .
C6 C7 1.45(2) .
C9 C10 1.41(2) .
C9 C14 1.415(19) .
C10 C11 1.35(2) .
C11 C12 1.38(2) .
C12 C13 1.40(2) .
C13 C14 1.42(2) .
C13 C16 1.43(2) .
C14 C15 1.41(2) .
