Synthesis and Structures of Lead(II) Complexes with Substituted Derivatives of the <i>Closo</i>-Decaborate Anion with a Pendant N<sub>3</sub> Group.
Matveev, Evgenii Yu; Dontsova, Olga S.; Avdeeva, Varvara V.; Kubasov, Alexey S.; Zhdanov, Andrey P.; Nikiforova, Svetlana E.; Goeva, Lyudmila V.; Zhizhin, Konstantin Yu; Malinina, Elena A.; Kuznetsov, Nikolay T.; Molecules (Basel, Switzerland) 28 (2023) 8073–; doi:10.3390/molecules28248073

data_1570721
_publ_section_title
;
 Synthesis and Structures of Lead(II) Complexes with Substituted
 Derivatives of the <i>Closo</i>-Decaborate Anion with a Pendant
 N<sub>3</sub> Group.
;
_journal_issue                   24
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              8073
_journal_paper_doi               10.3390/molecules28248073
_journal_volume                  28
_journal_year                    2023
_chemical_formula_moiety
'C34 H37 B10 N11 O8 Pb2, 0.5(C2 H3 N), 0.125(O)'
_chemical_formula_sum            'C35 H38.5 B10 N11.5 O8.12 Pb2'
_chemical_formula_weight         1272.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-12-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.153(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8622(8)
_cell_length_b                   17.0582(8)
_cell_length_c                   18.2240(9)
_cell_measurement_reflns_used    4959
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.34
_cell_volume                     4951.8(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19673
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.045
_diffrn_reflns_theta_min         1.681
_exptl_absorpt_coefficient_mu    6.849
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1008 before and 0.0419 after correction.
The Ratio of minimum to maximum transmission is 0.6350.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       needle
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.449
_refine_diff_density_min         -1.699
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         9718
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0706
_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^)+(0.0762P)^2^+41.1011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6229
_reflns_number_total             9718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            7.cif
_cod_data_source_block           mo_23kub21_0m_a
_cod_original_formula_sum        'C35 H38.50 B10 N11.50 O8.12 Pb2'
_cod_database_code               1570721
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.341
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C3A
 1.48 with sigma of 0.02
 N1B-N2B
 1.2 with sigma of 0.02
 N2B-N3B
 1.14 with sigma of 0.02
 C3B-C5B
 1.52 with sigma of 0.02
 C5B-C3B
 1.52 with sigma of 0.02
 C5A-C3A
 1.52 with sigma of 0.02
 C11-C10
 1.48 with sigma of 0.02
 C21-C20
 1.48 with sigma of 0.01
 C5B-N4B
 1.48 with sigma of 0.01
 N4B-N5B
 1.19 with sigma of 0.01
 N4B-N6B
 2.32 with sigma of 0.02
 C5A-N4A
 1.48 with sigma of 0.01
 N6A-N5B
 1.14 with sigma of 0.01
 N5B-N4A
 1.19 with sigma of 0.01
 N6A-N4A
 2.32 with sigma of 0.01
 N5B-N4B
 1.19 with sigma of 0.01
 N4A-N5A
 1.19 with sigma of 0.01
 N6A-N5A
 1.14 with sigma of 0.01
 N5B-N6B
 1.14 with sigma of 0.01
 C3A-N4A
 2.49 with sigma of 0.02
 C3B-N1B
 2.49 with sigma of 0.02
 C3B-C4B
 1.52 with sigma of 0.02
 C4B-N1B
 1.48 with sigma of 0.01
 N1B-C3B
 2.49 with sigma of 0.02
 N1B-N3B
 2.32 with sigma of 0.01
 C4A-C3A
 1.52 with sigma of 0.02
 N1A-C4A
 1.48 with sigma of 0.01
 N1A-N2A
 1.19 with sigma of 0.01
 N2A-N3A
 1.14 with sigma of 0.01
 C5B-N5B
 2.32 with sigma of 0.01
 C4B-N2B
 2.32 with sigma of 0.01
 C5A-N5A
 2.32 with sigma of 0.01
 C4A-N2A
 2.32 with sigma of 0.01
 C3B-N4B
 2.5 with sigma of 0.02
 C1-C2
 1.52 with sigma of 0.02
 C2-O2
 1.48 with sigma of 0.02
 B6-B9
 1.72 with sigma of 0.02
 C3A-N6A
 3.5 with sigma of 0.02
 B7-H7A
 1.12 with sigma of 0.01
 B8-H8A
 1.12 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N12) = Uanis(C25) = Uanis(C24) = Uanis(C23) = Uanis(C22) = Uanis(C21) =
Uanis(C20) = Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(N11)
Uanis(C26) = Uanis(N13) = Uanis(C30) = Uanis(C29) = Uanis(C28) = Uanis(C27) =
Uanis(N14) = Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35)
Uanis(O7B) = Uanis(O6B) = Uanis(O8B) = Uanis(O7A) = Uanis(O6A) = Uanis(O8A) =
Uanis(N10B) = Uanis(N10A)
Uanis(N9) = Uanis(C11) = Uanis(C15) = Uanis(C14) = Uanis(C12) = Uanis(C13) =
Uanis(N8) = Uanis(C10) = Uanis(C9) = Uanis(C6) = Uanis(C8) = Uanis(C7)
Uanis(B8) = Uanis(B2) = Uanis(B3) = Uanis(B4) = Uanis(B9) = Uanis(B6) =
Uanis(B10) = Uanis(B7) = Uanis(B1)
Uanis(C1) = Uanis(C2) = Uanis(O2)
Uanis(C4B) = Uanis(N1B)
Uanis(N5B) = Uanis(C5B)
Uanis(C5A) = Uanis(C5B)
Uanis(O5A) = Uanis(O3A) = Uanis(O4A) = Uanis(N7A) = Uanis(O3B) = Uanis(O4B) =
Uanis(O5B) = Uanis(N7B)
Uanis(C5B) = Uanis(N5B) = Uanis(C5A) = Uanis(N4B) = Uanis(N6B) = Uanis(N4A) =
Uanis(N6A)
Uanis(C5B) = Uanis(C5A) = Uanis(C3A) = Uanis(C3B)
Uanis(N5A) = Uanis(N5B)
Uanis(C4B) = Uanis(N1B) = Uanis(N3B) = Uanis(C4A) = Uanis(N1A) = Uanis(N3A) =
Uanis(N2A) = Uanis(N2B)
Uanis(C4B) = Uanis(C5A)
Uanis(C36) = Uanis(C37) = Uanis(N15)
4. Others
 Fixed Sof: O3A(0.4) O3B(0.6) O4B(0.6) O5B(0.6) N7B(0.6) O4A(0.4) O5A(0.4)
 O6A(0.5) O6B(0.5) O7A(0.5) O7B(0.5) O8A(0.5) O8B(0.5) N1A(0.2) N1B(0.3)
 N2A(0.2) N2B(0.3) N3A(0.2) N3B(0.3) N4A(0.2) N4B(0.3) N5A(0.2) N5B(0.3)
 N6A(0.2) N6B(0.3) N7A(0.4) N10A(0.5) N10B(0.5) C3A(0.4) C3B(0.6) C4A(0.2)
 C4B(0.3) C5A(0.2) C5B(0.3) C36(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5)
 O9B(0.125)
5.a Free rotating group:
 O3B(O4B,O5B,N7B)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C24(H24), C23(H23), C22(H22), C32(H32), C33(H33), C34(H34),
 C35(H35), C9(H9), C8(H8), C7(H7), C6(H6), C15(H15), C14(H14), C13(H13),
 C12(H12), C19(H19), C18(H18), C17(H17), C16(H16), C26(H26), C29(H29), C28(H28),
  C27(H27)
5.d Fitted hexagon refined as free rotating group:
 N12(C25,C24,C23,C22,C21), N14(C31,C32,C33,C34,C35), C10(C9,C8,C7,C6,N8),
 C11(N9,C15,C14,C13,C12), C20(C19,C18,C17,C16,N11), C26(N13,C30,C29,C28,C27)
5.e Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
5.f Boron cage BH refined with riding coordinates:
 B1(H1), B3(H3), B4(H4), B5(H5), B6(H6A), B9(H9A), B10(H10)
;
_shelx_res_checksum              99761
_shelx_hkl_checksum              88504
_olex2_submission_special_instructions 'No special instructions were received'