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_1570719
_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         'C28 H33 B10 N7 O2 Pb'
_chemical_formula_sum            'C28 H33 B10 N7 O2 Pb'
_chemical_formula_weight         814.90
_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   geom
_audit_creation_date             2023-11-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                73.72(2)
_cell_angle_beta                 87.76(2)
_cell_angle_gamma                88.16(2)
_cell_formula_units_Z            4
_cell_length_a                   11.273(5)
_cell_length_b                   13.638(8)
_cell_length_c                   22.354(14)
_cell_measurement_reflns_used    8053
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      29.188
_cell_measurement_theta_min      2.353
_cell_volume                     3296(3)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.1642
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30205
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.530
_diffrn_reflns_theta_min         1.580
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.160
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1101 before and 0.0471 after correction.
The Ratio of minimum to maximum transmission is 0.5928.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         8.672
_refine_diff_density_min         -3.763
_refine_diff_density_rms         0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         18856
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0797
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11994
_reflns_number_total             18856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4.cif
_cod_data_source_block           mo_23kub18_0m_a
_cod_database_code               1570719
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Others
 Fixed Sof: O4A(0.65) O4B(0.35) N8A(0.65) N8B(0.35) N9A(0.65) N9B(0.35)
 N10A(0.65) N10B(0.35) H27A(0.65) H27B(0.65) H27C(0.35) H27D(0.35) C28A(0.65)
 H28A(0.65) H28B(0.65) C28B(0.35) H28C(0.35) H28D(0.35) C29A(0.65) H29A(0.65)
 H29B(0.65) C29B(0.35) H29C(0.35) H29D(0.35) C30A(0.65) H30A(0.65) H30B(0.65)
 C30B(0.35) H30C(0.35) H30D(0.35)
 Fixed Uiso: H27A(0.035) H27B(0.035) H27C(0.035) H27D(0.035) H28A(0.056)
 H28B(0.056) H28C(0.056) H28D(0.056) H29A(0.064) H29B(0.064) H29C(0.064)
 H29D(0.064) H30A(0.115) H30B(0.115) H30C(0.115) H30D(0.115) H31(0.028)
 H32(0.043) H33(0.038) H35(0.042) H36(0.039) H38(0.037) H39(0.036) H40(0.032)
 H43(0.037) H44(0.043) H45(0.036) H47(0.037) H48(0.042) H50(0.039) H51(0.034)
 H52(0.03) H11(0.032) H13(0.031) H14(0.034) H15(0.032) H16(0.029) H17(0.029)
 H18(0.027) H19(0.031) H20(0.026) H1A(0.031) H1B(0.031) H2A(0.028) H2B(0.028)
 H3A(0.052) H3B(0.052) H4A(0.057) H4B(0.057) H5(0.034) H6(0.043) H7(0.049)
 H9(0.045) H10(0.04) H12(0.041) H13A(0.033) H14A(0.031) H17A(0.029) H18A(0.034)
 H19A(0.038) H21(0.042) H22(0.037) H24(0.039) H25(0.038) H26(0.033) H1(0.031)
 H3(0.029) H4(0.028) H5A(0.022) H6A(0.024) H7A(0.029) H8(0.027) H9A(0.022)
 H10A(0.024)
 Fixed X: H27A(0.367868) H27B(0.425925) H27C(0.385324) H27D(0.417451)
 H28A(0.236096) H28B(0.17546) H28C(0.243798) H28D(0.182125) H29A(0.114822)
 H29B(0.084059) H29C(0.043766) H29D(0.03291) H30A(-0.047969) H30B(0.027563)
 H30C(-0.046881) H30D(0.082522) H31(0.479569) H32(0.639825) H33(0.832318)
 H35(0.970079) H36(0.995065) H38(0.910435) H39(0.741508) H40(0.554561)
 H43(0.210146) H44(0.193268) H45(0.344109) H47(0.532483) H48(0.676391)
 H50(0.760839) H51(0.749958) H52(0.609705) H11(0.299302) H13(0.079147)
 H14(0.162408) H15(0.434057) H16(0.141932) H17(0.014277) H18(0.265325)
 H19(0.39536) H20(0.162305) H1A(0.425774) H1B(0.450864) H2A(0.299194)
 H2B(0.220049) H3A(0.106497) H3B(0.126173) H4A(0.032879) H4B(-0.054738)
 H5(0.451394) H6(0.595171) H7(0.79572) H9(0.949695) H10(0.99622) H12(0.930976)
 H13A(0.776254) H14A(0.580881) H17A(0.635839) H18A(0.777956) H19A(0.745649)
 H21(0.609354) H22(0.429745) H24(0.228862) H25(0.09308) H26(0.149781)
 H1(0.333338) H3(0.099604) H4(0.2128) H5A(0.470995) H6A(0.141583) H7A(0.042083)
 H8(0.302377) H9A(0.402176) H10A(0.1739)
 Fixed Y: H27A(0.421576) H27B(0.322535) H27C(0.419264) H27D(0.315415)
 H28A(0.282437) H28B(0.371454) H28C(0.291682) H28D(0.390883) H29A(0.195199)
 H29B(0.309075) H29C(0.345297) H29D(0.256688) H30A(0.190933) H30B(0.247112)
 H30C(0.205501) H30D(0.216514) H31(0.194392) H32(0.112542) H33(0.146636)
 H35(0.253099) H36(0.382646) H38(0.518254) H39(0.603396) H40(0.542147)
 H43(0.164478) H44(-0.006017) H45(-0.121703) H47(-0.155283) H48(-0.099194)
 H50(0.040761) H51(0.212047) H52(0.320113) H11(0.598401) H13(0.525968)
 H14(0.76805) H15(0.693699) H16(0.45683) H17(0.67622) H18(0.792151)
 H19(0.570229) H20(0.63588) H1A(0.583593) H1B(0.689398) H2A(0.709662)
 H2B(0.628769) H3A(0.779828) H3B(0.66393) H4A(0.708322) H4B(0.718118)
 H5(0.822735) H6(0.917525) H7(0.886678) H9(0.773608) H10(0.645573)
 H12(0.500954) H13A(0.411646) H14A(0.466776) H17A(0.709273) H18A(0.83272)
 H19A(0.997485) H21(1.121304) H22(1.1573) H24(1.096761) H25(0.96347)
 H26(0.803289) H1(0.43006) H3(0.483587) H4(0.252085) H5A(0.329297)
 H6A(0.537609) H7A(0.315895) H8(0.207192) H9A(0.429747) H10A(0.348095)
 Fixed Z: H27A(0.515258) H27B(0.499408) H27C(0.514086) H27D(0.496863)
 H28A(0.549519) H28B(0.495701) H28C(0.558216) H28D(0.512602) H29A(0.423848)
 H29B(0.426844) H29C(0.450118) H29D(0.514788) H30A(0.494389) H30B(0.534082)
 H30C(0.4294) H30D(0.396297) H31(0.238435) H32(0.20091) H33(0.220257)
 H35(0.261648) H36(0.306338) H38(0.349876) H39(0.375279) H40(0.365689)
 H43(0.305638) H44(0.308394) H45(0.35432) H47(0.412464) H48(0.464567)
 H50(0.499984) H51(0.501459) H52(0.444266) H11(0.498697) H13(0.457837)
 H14(0.413567) H15(0.383209) H16(0.345755) H17(0.338303) H18(0.288452)
 H19(0.296094) H20(0.238119) H1A(-0.007123) H1B(0.007232) H2A(-0.066644) H2B(-
 0.016435) H3A(0.064784) H3B(0.062982) H4A(-0.035438) H4B(0.021037)
 H5(0.253792) H6(0.284327) H7(0.262869) H9(0.230095) H10(0.185521)
 H12(0.145478) H13A(0.119441) H14A(0.133477) H17A(0.051377) H18A(0.013154)
 H19A(0.022099) H21(0.062961) H22(0.103194) H24(0.148764) H25(0.183325)
 H26(0.175508) H1(-0.005846) H3(0.043307) H4(0.070758) H5A(0.104477)
 H6A(0.160423) H7A(0.156327) H8(0.199892) H9A(0.202811) H10A(0.2613)
;
_shelx_res_checksum              6185
_shelx_hkl_checksum              24436
_olex2_submission_special_instructions 'No special instructions were received'