Pentazolate coordination polymers self-assembled by in situ generated [Pb4(OH)4]4+ cubic cations trapping cyclo-N5−
Yuan, Yuan; Xu, Yuangang; Xie, Qiang; Li, Dongxue; Lin, Qiuhan; Wang, Pengcheng; Lu, Ming; Dalton Transactions  (2022) –; doi:10.1039/D1DT04392G

data_7709691
_publ_section_title
;
 Pentazolate coordination polymers self-assembled by in situ generated
 [Pb4(OH)4]4+ cubic cations trapping cyclo-N5&#x2212;
;
_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       '\f and \w 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/[\s^2^(Fo^2^)+(0.0178P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            d1dt04392g2.cif
_cod_data_source_block           1_a
_cod_database_code               7709691
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.527
_shelx_estimated_absorpt_t_max   0.527
_shelx_res_checksum              38645