#------------------------------------------------------------------------------
#$Date: 2022-03-09 01:51:30 +0200 (Wed, 09 Mar 2022) $
#$Revision: 273541 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/96/7709690.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_7709690
loop_
_publ_author_name
'Yuan, Yuan'
'Xu, Yuangang'
'Xie, Qiang'
'Li, Dongxue'
'Lin, Qiuhan'
'Wang, Pengcheng'
'Lu, Ming'
_publ_section_title
;
 Pentazolate coordination polymers self-assembled by in situ generated
 [Pb4(OH)4]4+ cubic cations trapping cyclo-N5−
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04392G
_journal_year                    2022
_chemical_formula_moiety
'2(H18 N16 O12 Pb3), 4(N5), H3 O1.50, 2(O0.50), 2(H)'
_chemical_formula_sum            'H41 N52 O26.5 Pb6'
_chemical_formula_weight         2436.99
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-28 deposited with the CCDC.	2022-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   14.9624(5)
_cell_length_b                   14.9624(5)
_cell_length_c                   7.3194(2)
_cell_measurement_reflns_used    7396
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.72
_cell_volume                     1419.09(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14760
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         3.144
_diffrn_source.source            'Ius 2.0'
_diffrn_source.type              microfocus
_exptl_absorpt_coefficient_mu    17.850
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.852
_exptl_crystal_description       needle
_exptl_crystal_F_000             1109
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.766
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0160P)²+3.8176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1039
_reflns_number_total             1172
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt04392g2.cif
_cod_data_source_block           YY210323_a
_cod_original_cell_volume        1419.09(10)
_cod_original_formula_sum        'H41 N52 O26.50 Pb6'
_cod_database_code               7709690
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.125
_shelx_estimated_absorpt_t_max   0.842
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.49955(2) 0.58062(2) 0.250000 0.02420(8) Uani 1 2 d S T P . .
N1 N 0.5042(2) 0.3426(2) 0.3957(4) 0.0227(6) Uani 1 1 d . . . . .
N2 N 0.4943(3) 0.2542(2) 0.3403(4) 0.0272(7) Uani 1 1 d . . . . .
N3 N 0.5106(3) 0.3963(3) 0.250000 0.0196(9) Uani 1 2 d S T P . .
N4 N 0.333333 0.666667 0.250000 0.0219(16) Uani 1 6 d S T P . .
O3 O 0.3066(3) 0.5729(3) 0.250000 0.0326(9) Uani 1 2 d S T P . .
O1 O 0.6646(4) 0.7653(4) 0.250000 0.0607(14) Uani 1 2 d S T P . .
H1A H 0.646631 0.810998 0.250000 0.091 Uiso 1 2 d R U P . .
H1B H 0.696981 0.774728 0.149970 0.091 Uiso 0.5 1 d R U P . .
O2 O 0.37214(19) 0.4332(2) 0.0053(4) 0.0276(6) Uani 1 1 d . . . . .
H2A H 0.324731 0.376466 0.071517 0.041 Uiso 1 1 d R U . . .
H2B H 0.328741 0.449936 -0.044883 0.041 Uiso 1 1 d R U . . .
N5 N 0.1397(9) 0.2239(10) 0.750000 0.073(3) Uani 0.6667 2 d S T P A 1
N6 N 0.0239(5) 0.2581(6) 0.6640(11) 0.0547(18) Uani 0.6667 1 d . . P A 1
N7 N 0.0988(7) 0.2400(7) 0.6077(12) 0.082(3) Uani 0.6667 1 d . . P A 1
O4 O -0.0212(18) 0.2581(16) 0.750000 0.048(5) Uani 0.25 2 d S T P B 2
H4 H -0.034378 0.224183 0.849080 0.072 Uiso 0.25 1 d R U P B 2
O5 O 1.000000 1.000000 0.500000 0.126(12) Uani 0.5 6 d S T P . .
H5A H 1.036790 0.973530 0.528920 0.188 Uiso 0.0833 1 d R U P . .
H5B H 0.938230 0.950990 0.512490 0.188 Uiso 0.0833 1 d R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'
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
O1 Pb1 O2 139.14(6) . 12_556 ?
O1 Pb1 O2 139.14(6) . . ?
O2 Pb1 O2 81.66(11) 12_556 . ?
N3 N1 N2 107.6(3) . . ?
N1 N2 N2 107.91(19) . 12_556 ?
N1 N3 N1 109.0(4) 12_556 . ?
O3 N4 O3 119.996(1) 8_566 9_666 ?
O3 N4 O3 120.001(1) 8_566 . ?
O3 N4 O3 120.003(1) 9_666 . ?
Pb1 O1 H1A 109.7 . . ?
Pb1 O1 H1B 109.4 . . ?
H1A O1 H1B 104.5 . . ?
Pb1 O1 H1B 109.39(5) . 12_556 ?
H1A O1 H1B 104.5 . 12_556 ?
H1B O1 H1B 118.9 . 12_556 ?
Pb1 O2 H2A 107.6 . . ?
Pb1 O2 H2B 111.0 . . ?
H2A O2 H2B 98.2 . . ?
N7 N5 N7 107.7(10) . 12_557 ?
N6 N6 N7 107.9(5) 12_557 . ?
N6 N6 H4 97.2(5) 12_557 12_557 ?
N7 N6 H4 128.1(16) . 12_557 ?
N5 N7 N6 108.1(8) . . ?
H5A O5 H5B 104.4 . . ?
H5A O5 H5A 180.0 . 7_776 ?
H5B O5 H5A 75.6 . 7_776 ?
H5A O5 H5A 114.0 . 4_765 ?
H5B O5 H5A 129.4 . 4_765 ?
H5A O5 H5A 66.0 7_776 4_765 ?
H5A O5 H5A 66.0 . 10_566 ?
H5B O5 H5A 50.6 . 10_566 ?
H5A O5 H5A 114.0 7_776 10_566 ?
H5A O5 H5A 180.0 4_765 10_566 ?
H5A O5 H5A 114.0 . 5_675 ?
H5B O5 H5A 15.5 . 5_675 ?
H5A O5 H5A 66.0 7_776 5_675 ?
H5A O5 H5A 114.0 4_765 5_675 ?
H5A O5 H5A 66.0 10_566 5_675 ?
H5A O5 H5A 66.0 . 11_656 ?
H5B O5 H5A 164.5 . 11_656 ?
H5A O5 H5A 114.0 7_776 11_656 ?
H5A O5 H5A 66.0 4_765 11_656 ?
H5A O5 H5A 114.0 10_566 11_656 ?
H5A O5 H5A 180.0 5_675 11_656 ?
H5A O5 H5B 75.6 . 7_776 ?
H5B O5 H5B 180.0 . 7_776 ?
H5A O5 H5B 104.4 7_776 7_776 ?
H5A O5 H5B 50.6 4_765 7_776 ?
H5A O5 H5B 129.4 10_566 7_776 ?
H5A O5 H5B 164.5 5_675 7_776 ?
H5A O5 H5B 15.5 11_656 7_776 ?
H5A O5 H5B 15.5 . 4_765 ?
H5B O5 H5B 118.9 . 4_765 ?
H5A O5 H5B 164.5 7_776 4_765 ?
H5A O5 H5B 104.4 4_765 4_765 ?
H5A O5 H5B 75.6 10_566 4_765 ?
H5A O5 H5B 129.4 5_675 4_765 ?
H5A O5 H5B 50.6 11_656 4_765 ?
H5B O5 H5B 61.1 7_776 4_765 ?
H5A O5 H5B 164.5 . 10_566 ?
H5B O5 H5B 61.1 . 10_566 ?
H5A O5 H5B 15.5 7_776 10_566 ?
H5A O5 H5B 75.6 4_765 10_566 ?
H5A O5 H5B 104.4 10_566 10_566 ?
H5A O5 H5B 50.6 5_675 10_566 ?
H5A O5 H5B 129.4 11_656 10_566 ?
H5B O5 H5B 118.9 7_776 10_566 ?
H5B O5 H5B 180.0 4_765 10_566 ?
H5A O5 H5B 129.4 . 5_675 ?
H5B O5 H5B 118.9 . 5_675 ?
H5A O5 H5B 50.6 7_776 5_675 ?
H5A O5 H5B 15.5 4_765 5_675 ?
H5A O5 H5B 164.5 10_566 5_675 ?
H5A O5 H5B 104.4 5_675 5_675 ?
H5A O5 H5B 75.6 11_656 5_675 ?
H5B O5 H5B 61.1 7_776 5_675 ?
H5B O5 H5B 118.9 4_765 5_675 ?
H5B O5 H5B 61.1 10_566 5_675 ?
H5A O5 H5B 50.6 . 11_656 ?
H5B O5 H5B 61.1 . 11_656 ?
H5A O5 H5B 129.4 7_776 11_656 ?
H5A O5 H5B 164.5 4_765 11_656 ?
H5A O5 H5B 15.5 10_566 11_656 ?
H5A O5 H5B 75.6 5_675 11_656 ?
H5A O5 H5B 104.4 11_656 11_656 ?
H5B O5 H5B 118.9 7_776 11_656 ?
H5B O5 H5B 61.1 4_765 11_656 ?
H5B O5 H5B 118.9 10_566 11_656 ?
H5B O5 H5B 180.0 5_675 11_656 ?
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 O1 2.629(5) . ?
Pb1 O2 2.739(3) 12_556 ?
Pb1 O2 2.739(3) . ?
N1 N3 1.310(4) . ?
N1 N2 1.319(4) . ?
N2 N2 1.322(6) 12_556 ?
N4 O3 1.252(4) 8_566 ?
N4 O3 1.252(4) 9_666 ?
N4 O3 1.252(4) . ?
O1 H1A 0.8500 . ?
O1 H1B 0.8500 . ?
O1 H1B 0.8501 12_556 ?
O2 H2A 0.9254 . ?
O2 H2B 0.8843 . ?
N5 N7 1.290(10) . ?
N5 N7 1.290(10) 12_557 ?
N6 N6 1.258(15) 12_557 ?
N6 N7 1.344(10) . ?
N6 H4 0.76(2) 12_557 ?
O4 H4 0.8500 . ?
O4 H4 0.8501 12_557 ?
O5 H5A 0.8501 . ?
O5 H5B 0.8500 . ?
O5 H5A 0.8502 7_776 ?
O5 H5A 0.8502 4_765 ?
O5 H5A 0.8502 10_566 ?
O5 H5A 0.8502 5_675 ?
O5 H5A 0.8502 11_656 ?
O5 H5B 0.8500 7_776 ?
O5 H5B 0.8500 4_765 ?
O5 H5B 0.8500 10_566 ?
O5 H5B 0.8500 5_675 ?
O5 H5B 0.8500 11_656 ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 N1 N2 N2 -0.3(3) . . . 12_556 ?
N2 N1 N3 N1 0.4(5) . . . 12_556 ?
N7 N5 N7 N6 -5.3(16) 12_557 . . . ?
N6 N6 N7 N5 3.3(10) 12_557 . . . ?
