#------------------------------------------------------------------------------
#$Date: 2022-03-09 01:51:30 +0200 (Wed, 09 Mar 2022) $
#$Revision: 273541 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/96/7709691.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_7709691
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         'Cl H6 N15 O9 Pb4'
_chemical_formula_sum            'Cl H6 N15 O9 Pb4'
_chemical_formula_weight         1224.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_formula_units_Z            4
_cell_length_a                   10.1088(8)
_cell_length_b                   13.5520(11)
_cell_length_c                   13.4401(9)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.51
_cell_volume                     1841.2(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0655
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17903
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.594
_diffrn_reflns_theta_min         2.935
_diffrn_source.source            'Ius 2.0'
_diffrn_source.type              microfocus
_exptl_absorpt_coefficient_mu    36.686
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.417
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.225
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.034(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3982
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0275
_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)+(0.0178P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.790
_reflns_Friedel_fraction_full    0.917
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                3669
_reflns_number_total             3982
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt04392g2.cif
_cod_data_source_block           1_a
_cod_database_code               7709691
_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   0.527
_shelx_estimated_absorpt_t_max   0.527
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'
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 0.78990(5) 0.35207(3) 0.25098(4) 0.02531(13) Uani 1 1 d . . . . .
Pb2 Pb 1.14069(5) 0.29182(4) 0.34914(4) 0.02577(13) Uani 1 1 d . . . . .
Pb3 Pb 1.03794(5) 0.20994(4) 0.08328(4) 0.02620(13) Uani 1 1 d . . . . .
Pb4 Pb 0.88389(5) 0.08651(4) 0.31274(4) 0.02916(14) Uani 1 1 d . . . . .
N1 N 0.9138(12) 0.4833(9) 0.3774(9) 0.031(3) Uani 1 1 d . . . . .
N2 N 1.0437(12) 0.4845(8) 0.3793(8) 0.030(3) Uani 1 1 d . . . . .
N3 N 1.0820(13) 0.5640(9) 0.4256(10) 0.035(3) Uani 1 1 d . . . . .
N4 N 0.9761(13) 0.6118(9) 0.4533(10) 0.035(3) Uani 1 1 d . . . . .
N5 N 0.8705(12) 0.5628(9) 0.4234(10) 0.034(3) Uani 1 1 d . . . . .
N6 N 0.5469(12) 0.5923(10) 0.5891(11) 0.038(3) Uani 1 1 d . . . . .
N7 N 0.6086(16) 0.5530(12) 0.6657(12) 0.055(4) Uani 1 1 d . . . . .
N8 N 0.7196(14) 0.6040(11) 0.6772(11) 0.049(4) Uani 1 1 d . . . . .
N9 N 0.7265(12) 0.6730(10) 0.6086(9) 0.031(3) Uani 1 1 d . . . . .
N10 N 0.6185(13) 0.6642(10) 0.5550(10) 0.037(3) Uani 1 1 d . . . . .
N11 N 0.8475(15) 0.8835(10) -0.0192(10) 0.043(3) Uani 1 1 d . . . . .
N12 N 0.9438(16) 0.9482(10) -0.0238(10) 0.045(4) Uani 1 1 d . . . . .
N13 N 0.9310(16) 1.0099(10) 0.0516(10) 0.048(4) Uani 1 1 d . . . . .
N14 N 0.8270(16) 0.9802(11) 0.1021(12) 0.057(4) Uani 1 1 d . . . . .
N15 N 0.7765(14) 0.9036(9) 0.0591(12) 0.050(4) Uani 1 1 d . . . . .
O1 O 0.8287(9) 0.1915(6) 0.1798(7) 0.028(2) Uani 1 1 d . . . . .
H1A H 0.754509 0.167209 0.139679 0.034 Uiso 1 1 calc R U . . .
O2 O 0.9144(9) 0.2498(6) 0.3722(7) 0.025(2) Uani 1 1 d . . . . .
H2A H 0.884236 0.258711 0.440925 0.031 Uiso 1 1 calc R U . . .
O3 O 1.0061(9) 0.3422(6) 0.2020(7) 0.024(2) Uani 1 1 d . . . . .
H3A H 1.036881 0.405342 0.174963 0.028 Uiso 1 1 calc R U . . .
O4 O 1.0837(9) 0.1451(6) 0.2443(7) 0.0235(19) Uani 1 1 d . . . . .
H4A H 1.153605 0.095008 0.243719 0.028 Uiso 1 1 calc R U . . .
Cl1 Cl 0.4716(4) 0.8347(3) 0.8044(3) 0.0366(8) Uani 1 1 d . . . . .
O5 O 0.4762(14) 0.7583(11) 0.7321(13) 0.077(5) Uani 1 1 d . . . . .
O6 O 0.5978(10) 0.8460(9) 0.8512(11) 0.052(3) Uani 1 1 d . . . . .
O7 O 0.4331(12) 0.9264(9) 0.7599(11) 0.054(3) Uani 1 1 d . . . . .
O8 O 0.3730(11) 0.8098(9) 0.8789(10) 0.053(3) Uani 1 1 d . . . . .
O9 O 0.7222(11) 0.3540(9) 0.0524(9) 0.052(3) Uani 1 1 d . . . . .
H9A H 0.781053 0.378356 0.014507 0.077 Uiso 1 1 d R U . . .
H9B H 0.654513 0.389956 0.042907 0.077 Uiso 1 1 d R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 '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
O3 Pb1 O1 71.2(3) . . ?
O3 Pb1 O2 70.8(3) . . ?
O1 Pb1 O2 71.0(3) . . ?
O3 Pb1 O9 87.7(3) . . ?
O1 Pb1 O9 70.4(3) . . ?
O2 Pb1 O9 140.1(3) . . ?
O3 Pb1 N1 77.3(4) . . ?
O1 Pb1 N1 138.8(3) . . ?
O2 Pb1 N1 74.1(3) . . ?
O9 Pb1 N1 134.7(3) . . ?
O2 Pb2 O3 69.2(3) . . ?
O2 Pb2 O4 70.2(3) . . ?
O3 Pb2 O4 69.3(3) . . ?
O4 Pb3 O3 72.6(3) . . ?
O4 Pb3 O1 69.8(3) . . ?
O3 Pb3 O1 67.6(3) . . ?
O1 Pb4 O4 72.7(3) . . ?
O1 Pb4 O2 73.9(3) . . ?
O4 Pb4 O2 72.9(3) . . ?
N2 N1 N5 108.2(11) . . ?
N2 N1 Pb1 118.3(8) . . ?
N5 N1 Pb1 131.7(9) . . ?
N3 N2 N1 108.5(11) . . ?
N2 N3 N4 107.6(12) . . ?
N3 N4 N5 109.1(12) . . ?
N1 N5 N4 106.6(11) . . ?
N10 N6 N7 108.4(13) . . ?
N6 N7 N8 106.3(13) . . ?
N9 N8 N7 109.5(13) . . ?
N10 N9 N8 106.1(12) . . ?
N6 N10 N9 109.7(12) . . ?
N15 N11 N12 107.9(12) . . ?
N11 N12 N13 108.3(13) . . ?
N14 N13 N12 106.3(13) . . ?
N15 N14 N13 109.4(14) . . ?
N14 N15 N11 108.2(13) . . ?
Pb4 O1 Pb1 106.4(4) . . ?
Pb4 O1 Pb3 104.8(3) . . ?
Pb1 O1 Pb3 104.7(3) . . ?
Pb4 O2 Pb2 107.7(3) . . ?
Pb4 O2 Pb1 103.5(3) . . ?
Pb2 O2 Pb1 105.6(3) . . ?
Pb1 O3 Pb3 111.1(4) . . ?
Pb1 O3 Pb2 108.0(4) . . ?
Pb3 O3 Pb2 104.3(3) . . ?
Pb4 O4 Pb3 108.2(3) . . ?
Pb4 O4 Pb2 104.2(3) . . ?
Pb3 O4 Pb2 105.2(3) . . ?
O5 Cl1 O6 110.5(9) . . ?
O5 Cl1 O7 110.8(10) . . ?
O6 Cl1 O7 109.4(7) . . ?
O5 Cl1 O8 109.0(8) . . ?
O6 Cl1 O8 109.5(8) . . ?
O7 Cl1 O8 107.6(8) . . ?
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 O3 2.286(9) . ?
Pb1 O1 2.410(9) . ?
Pb1 O2 2.482(9) . ?
Pb1 O9 2.755(12) . ?
Pb1 N1 2.760(12) . ?
Pb2 O2 2.378(9) . ?
Pb2 O3 2.496(9) . ?
Pb2 O4 2.504(9) . ?
Pb3 O4 2.381(9) . ?
Pb3 O3 2.422(9) . ?
Pb3 O1 2.494(10) . ?
Pb4 O1 2.351(10) . ?
Pb4 O4 2.357(9) . ?
Pb4 O2 2.373(9) . ?
N1 N2 1.313(16) . ?
N1 N5 1.318(17) . ?
N2 N3 1.303(17) . ?
N3 N4 1.306(17) . ?
N4 N5 1.320(17) . ?
N6 N10 1.298(18) . ?
N6 N7 1.32(2) . ?
N7 N8 1.326(19) . ?
N8 N9 1.314(18) . ?
N9 N10 1.314(17) . ?
N11 N15 1.303(19) . ?
N11 N12 1.312(19) . ?
N12 N13 1.320(18) . ?
N13 N14 1.314(19) . ?
N14 N15 1.292(19) . ?
Cl1 O5 1.419(14) . ?
Cl1 O6 1.432(12) . ?
Cl1 O7 1.434(12) . ?
Cl1 O8 1.453(12) . ?
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
N5 N1 N2 N3 -0.3(15) . . . . ?
Pb1 N1 N2 N3 166.3(9) . . . . ?
N1 N2 N3 N4 0.6(15) . . . . ?
N2 N3 N4 N5 -0.7(16) . . . . ?
N2 N1 N5 N4 -0.1(15) . . . . ?
Pb1 N1 N5 N4 -164.2(9) . . . . ?
N3 N4 N5 N1 0.5(16) . . . . ?
N10 N6 N7 N8 0.3(19) . . . . ?
N6 N7 N8 N9 -0.3(19) . . . . ?
N7 N8 N9 N10 0.2(18) . . . . ?
N7 N6 N10 N9 -0.2(18) . . . . ?
N8 N9 N10 N6 0.0(17) . . . . ?
N15 N11 N12 N13 -1(2) . . . . ?
N11 N12 N13 N14 1(2) . . . . ?
N12 N13 N14 N15 -1(2) . . . . ?
N13 N14 N15 N11 0(2) . . . . ?
N12 N11 N15 N14 1(2) . . . . ?
