Construction of efficient Pb(II) carboxylate catalysts for the oxygen and hydrogen evolution reactions.
Janak, ?; Sapner, Vijay S.; Sathe, Bhaskar R.; Khullar, Sadhika; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1087–1102; doi:10.1039/d4dt02958e

data_7717442
_publ_section_title
;
 Construction of efficient Pb(II) carboxylate catalysts for the oxygen and
 hydrogen evolution reactions.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1087
_journal_page_last               1102
_journal_paper_doi               10.1039/d4dt02958e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C23 H20 N3 O6 Pb), 4(H0.50 O0.25)'
_chemical_formula_sum            'C46 H45 N6 O14.5 Pb2'
_chemical_formula_weight         1328.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-17 deposited with the CCDC.	2024-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                111.089(4)
_cell_angle_beta                 93.623(4)
_cell_angle_gamma                90.726(4)
_cell_formula_units_Z            1
_cell_length_a                   10.3147(14)
_cell_length_b                   10.3481(15)
_cell_length_c                   12.0696(16)
_cell_measurement_reflns_used    9619
_cell_measurement_temperature    100.14(10)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.78
_cell_volume                     1198.7(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.14(10)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            49792
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.463
_diffrn_reflns_theta_min         2.111
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    7.086
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1385 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.6317.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             643
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4913
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.255
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0167
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+0.7109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4793
_reflns_number_total             4913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02958e2.cif
_cod_data_source_block           JC1
_cod_depositor_comments
'Adding full bibliography for 7717442--7717443.cif.'
_cod_original_formula_sum        'C46 H45 N6 O14.50 Pb2'
_cod_database_code               7717442
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Pb1-N2 \\sim Pb1-N3 \\sim Pb1-N1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.002
Uanis(C10) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O8(0.25) HB(0.25) HC(0.25)
 Fixed U11: O8(0.088482)
 Fixed U12: O8(-0.011377)
 Fixed U13: O8(-0.003705)
 Fixed U22: O8(0.080885)
 Fixed U23: O8(0.009276)
 Fixed U33: O8(0.07433)
5.a Free rotating group:
 O7(H,HA), O8(HB,HC)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C14(H14A,H14B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C19(H19), C21(H21)
5.d Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_shelx_res_checksum              77406
_shelx_hkl_checksum              46818
_olex2_submission_special_instructions 'No special instructions were received'