#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:14:46 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179620 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/84/4508454.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_4508454
loop_
_publ_author_name
'Yuan, Xiaoju'
'Zhang, Xiaoxia'
'Zhao, Hong'
'Liu, Lina'
'Wu, Benlai'
_publ_section_title
;
 Syntheses and Properties of One--Three-Dimensional Coordination Polymers
 Constructed by Metallohelicates of Purin-Containing Carboxylate
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4859
_journal_paper_doi               10.1021/cg401022z
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C14 H14 N8 O8 Pb'
_chemical_formula_weight         629.52
_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                 92.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.8998(14)
_cell_length_b                   9.2699(19)
_cell_length_c                   13.549(3)
_cell_measurement_reflns_used    1712
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.3106
_cell_measurement_theta_min      3.2534
_cell_volume                     865.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3338
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    9.815
_exptl_absorpt_correction_T_max  0.180
_exptl_absorpt_correction_T_min  0.121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.684
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0255
_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)+(0.0253P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                1160
_reflns_number_total             1520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401022z_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4508454
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 0.0000 0.5000 0.5000 0.02781(12) Uani 1 2 d S
N3 N 0.3143(6) 1.1101(5) 0.5255(4) 0.0241(11) Uani 1 1 d .
O1 O 0.0715(5) 0.7967(4) 0.3429(3) 0.0324(10) Uani 1 1 d .
C4 C 0.1457(7) 0.8814(5) 0.4014(4) 0.0202(12) Uani 1 1 d .
N4 N 0.1891(6) 1.0250(4) 0.3707(3) 0.0226(11) Uani 1 1 d .
N1 N 0.1870(6) 0.7397(5) 0.5595(4) 0.0267(11) Uani 1 1 d .
C3 C 0.1996(7) 0.8619(6) 0.5028(4) 0.0217(12) Uani 1 1 d .
C6 C 0.1374(8) 1.0626(6) 0.2687(4) 0.0270(13) Uani 1 1 d .
H6A H 0.1441 1.1688 0.2619 0.032 Uiso 1 1 calc R
H6B H 0.0010 1.0336 0.2540 0.032 Uiso 1 1 calc R
N2 N 0.3237(6) 0.9169(5) 0.6489(4) 0.0257(11) Uani 1 1 d .
H2 H 0.3777 0.9624 0.7001 0.031 Uiso 1 1 calc R
C2 C 0.2823(7) 0.9720(5) 0.5577(4) 0.0219(13) Uani 1 1 d .
C5 C 0.2652(7) 1.1276(6) 0.4333(4) 0.0228(13) Uani 1 1 d .
H5 H 0.2839 1.2210 0.4064 0.027 Uiso 1 1 calc R
C1 C 0.2653(8) 0.7782(6) 0.6450(5) 0.0296(14) Uani 1 1 d .
H1 H 0.2797 0.7142 0.6995 0.035 Uiso 1 1 calc R
O3 O 0.1866(6) 0.9886(4) 0.1062(3) 0.0385(11) Uani 1 1 d .
C7 C 0.2623(8) 0.9954(5) 0.1918(4) 0.0261(13) Uani 1 1 d .
O2 O 0.4283(5) 0.9494(4) 0.2147(3) 0.0332(10) Uani 1 1 d .
O4 O 0.2964(6) 0.3964(4) 0.6063(3) 0.0350(10) Uani 1 1 d D
H4A H 0.328(8) 0.311(2) 0.593(5) 0.052 Uiso 1 1 d D
H4B H 0.390(6) 0.443(5) 0.586(5) 0.052 Uiso 1 1 d 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
O4 Pb1 O4 180.0 . 3_566
O4 Pb1 O3 69.50(13) . 2_545
O4 Pb1 O3 110.50(13) 3_566 2_545
O4 Pb1 O3 110.50(13) . 4_576
O4 Pb1 O3 69.50(13) 3_566 4_576
O3 Pb1 O3 180.0 2_545 4_576
O4 Pb1 N1 102.38(13) . 3_566
O4 Pb1 N1 77.62(13) 3_566 3_566
O3 Pb1 N1 101.39(13) 2_545 3_566
O3 Pb1 N1 78.61(13) 4_576 3_566
O4 Pb1 N1 77.62(13) . .
O4 Pb1 N1 102.38(13) 3_566 .
O3 Pb1 N1 78.61(13) 2_545 .
O3 Pb1 N1 101.39(13) 4_576 .
N1 Pb1 N1 180.0(3) 3_566 .
C5 N3 C2 112.7(5) . .
O1 C4 C3 129.4(5) . .
O1 C4 N4 120.0(5) . .
C3 C4 N4 110.5(5) . .
C5 N4 C4 123.3(5) . .
C5 N4 C6 119.6(5) . .
C4 N4 C6 117.0(5) . .
C1 N1 C3 103.7(4) . .
C1 N1 Pb1 132.0(4) . .
C3 N1 Pb1 123.9(4) . .
C2 C3 N1 110.2(5) . .
C2 C3 C4 121.0(5) . .
N1 C3 C4 128.8(5) . .
N4 C6 C7 115.6(4) . .
N4 C6 H6A 108.4 . .
C7 C6 H6A 108.4 . .
N4 C6 H6B 108.4 . .
C7 C6 H6B 108.4 . .
H6A C6 H6B 107.4 . .
C1 N2 C2 105.9(5) . .
C1 N2 H2 127.1 . .
C2 N2 H2 127.1 . .
N2 C2 C3 106.2(5) . .
N2 C2 N3 127.6(5) . .
C3 C2 N3 126.1(5) . .
N3 C5 N4 126.2(5) . .
N3 C5 H5 116.9 . .
N4 C5 H5 116.9 . .
N1 C1 N2 114.0(5) . .
N1 C1 H1 123.0 . .
N2 C1 H1 123.0 . .
C7 O3 Pb1 100.6(3) . 2
O2 C7 O3 123.6(5) . .
O2 C7 C6 120.9(6) . .
O3 C7 C6 115.5(5) . .
Pb1 O4 H4A 116(5) . .
Pb1 O4 H4B 103(5) . .
H4A O4 H4B 101.4(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O4 2.629(4) .
Pb1 O4 2.629(4) 3_566
Pb1 O3 2.653(4) 2_545
Pb1 O3 2.653(4) 4_576
Pb1 N1 2.676(4) 3_566
Pb1 N1 2.676(4) .
N3 C5 1.290(7) .
N3 C2 1.374(6) .
O1 C4 1.213(6) .
C4 C3 1.418(8) .
C4 N4 1.430(6) .
N4 C5 1.363(7) .
N4 C6 1.455(7) .
N1 C1 1.305(7) .
N1 C3 1.374(6) .
C3 C2 1.372(7) .
C6 C7 1.516(8) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
N2 C1 1.348(7) .
N2 C2 1.354(7) .
N2 H2 0.8800 .
C5 H5 0.9500 .
C1 H1 0.9500 .
O3 C7 1.252(7) .
O3 Pb1 2.653(4) 2
C7 O2 1.249(7) .
O4 H4A 0.842(10) .
O4 H4B 0.835(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O2 0.88 1.91 2.756(6) 160.2 3_676
O4 H4B O3 0.835(10) 2.15(4) 2.896(6) 149(7) 4_676
O4 H4A N3 0.842(10) 2.08(3) 2.876(6) 158(6) 1_545
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
O1 C4 N4 C5 177.3(5) .
C3 C4 N4 C5 -2.1(6) .
O1 C4 N4 C6 0.9(7) .
C3 C4 N4 C6 -178.5(4) .
O4 Pb1 N1 C1 -43.9(5) .
O4 Pb1 N1 C1 136.1(5) 3_566
O3 Pb1 N1 C1 -115.1(5) 2_545
O3 Pb1 N1 C1 64.9(5) 4_576
N1 Pb1 N1 C1 85(75) 3_566
O4 Pb1 N1 C3 144.5(4) .
O4 Pb1 N1 C3 -35.5(4) 3_566
O3 Pb1 N1 C3 73.3(4) 2_545
O3 Pb1 N1 C3 -106.7(4) 4_576
N1 Pb1 N1 C3 -87(75) 3_566
C1 N1 C3 C2 -1.3(6) .
Pb1 N1 C3 C2 172.2(3) .
C1 N1 C3 C4 176.6(5) .
Pb1 N1 C3 C4 -9.9(7) .
O1 C4 C3 C2 -179.8(5) .
N4 C4 C3 C2 -0.4(7) .
O1 C4 C3 N1 2.5(9) .
N4 C4 C3 N1 -178.1(5) .
C5 N4 C6 C7 111.3(6) .
C4 N4 C6 C7 -72.2(6) .
C1 N2 C2 C3 0.1(6) .
C1 N2 C2 N3 179.7(5) .
N1 C3 C2 N2 0.8(6) .
C4 C3 C2 N2 -177.3(5) .
N1 C3 C2 N3 -178.8(4) .
C4 C3 C2 N3 3.1(8) .
C5 N3 C2 N2 177.6(5) .
C5 N3 C2 C3 -2.9(7) .
C2 N3 C5 N4 0.1(7) .
C4 N4 C5 N3 2.5(8) .
C6 N4 C5 N3 178.8(5) .
C3 N1 C1 N2 1.4(6) .
Pb1 N1 C1 N2 -171.4(3) .
C2 N2 C1 N1 -1.0(6) .
Pb1 O3 C7 O2 -29.2(6) 2
Pb1 O3 C7 C6 151.5(4) 2
N4 C6 C7 O2 -20.9(8) .
N4 C6 C7 O3 158.4(5) .
