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_1570720
_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         'C53 H51 B10 N13 O7 Pb2, 3(C2 H3 N)'
_chemical_formula_sum            'C59 H60 B10 N16 O7 Pb2'
_chemical_formula_weight         1627.71
_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     iterative
_audit_creation_date             2023-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                99.786(19)
_cell_angle_beta                 95.463(18)
_cell_angle_gamma                97.987(9)
_cell_formula_units_Z            2
_cell_length_a                   9.377(3)
_cell_length_b                   17.981(6)
_cell_length_c                   19.298(10)
_cell_measurement_reflns_used    7147
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.096
_cell_measurement_theta_min      2.158
_cell_volume                     3152(2)
_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      100.00
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18658
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.103
_diffrn_reflns_theta_max         25.103
_diffrn_reflns_theta_min         2.158
_exptl_absorpt_coefficient_mu    5.402
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0634 before and 0.0367 after correction.
The Ratio of minimum to maximum transmission is 0.8094.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.101
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         10974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0338P)^2^+23.7536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8876
_reflns_number_total             10974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6.cif
_cod_data_source_block           mo_22kub294_0m_a
_cod_database_code               1570720
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.813
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C59) = Uanis(C58) = Uanis(N16)
2. Others
 Fixed X: H3(0.42842) H5(0.622841) H6A(0.46146) H7A(0.18931) H8A(0.327841)
 H9(0.61005)
 Fixed Y: H3(0.155241) H5(0.151701) H6A(0.318261) H7A(0.18521) H8A(0.18503)
 H9(0.313931)
 Fixed Z: H3(0.118071) H5(0.348741) H6A(0.189321) H7A(0.20206) H8A(0.365281)
 H9(0.350161)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38),
 C39(H39), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50),
  C51(H51)
3.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C)
3.d Boron cage BH refined with riding coordinates:
 B1(H1), B4(H4), B10(H10A)
;
_shelx_res_checksum              19795
_shelx_hkl_checksum              93548
_olex2_submission_special_instructions 'No special instructions were received'