Introduction of plumbole to f-element chemistry
Münzfeld, Luca; Sun, Xiaofei; Schlittenhardt, Sören; Schoo, Christoph; Hauser, Adrian; Gillhuber, Sebastian; Weigend, Florian; Ruben, Mario; Roesky, Peter W.; Chemical Science 13 (2022) 945–954; doi:10.1039/D1SC03805B

data_1565670
_publ_section_title
;
 Introduction of plumbole to f-element chemistry
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              945
_journal_page_last               954
_journal_paper_doi               10.1039/D1SC03805B
_journal_volume                  13
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C58 H97 La Li O Pb Si4'
_chemical_formula_sum            'C58 H97 La Li O Pb Si4'
_chemical_formula_weight         1275.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-03
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2021-03-02 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.420(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4752(3)
_cell_length_b                   13.6204(2)
_cell_length_c                   16.9090(4)
_cell_measurement_reflns_used    93308
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      1.53
_cell_volume                     3061.59(11)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details
;
 1643 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52341
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.073
_diffrn_reflns_theta_min         1.532
_exptl_absorpt_coefficient_mu    3.547
_exptl_absorpt_correction_T_max  0.5636
_exptl_absorpt_correction_T_min  0.1305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1302
_exptl_crystal_size_max          0.673
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.791
_refine_diff_density_min         -1.624
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Flack x determined using 5912 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         15998
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0727P)^2^+7.3248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.855
_reflns_number_gt                14247
_reflns_number_total             15998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03805b2.cif
_cod_data_source_block           lmm137_repr
_cod_depositor_comments
'Adding full bibliography for 1565662--1565670.cif.'
_cod_database_code               1565670
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.199
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H15A,H15B,H15} of C15, {H16A,H16B,H16} of C16, All C(H,H)
  groups
 At 1.5 times of:
  {H45D,H45E,H45F} of C45A, {H49D,H49E,H49F} of C49B, {H51D,H51E,H51F} of
  C51A, {H48D,H48E,H48F} of C48B, {H46D,H46E,H46F} of C46A, {H40D,H40E,H40F} of
  C40B, {H25D,H25E,H25F} of C25A, {H23D,H23E,H23F} of C23A, {H26D,H26E,H26F} of
  C26A, {H42D,H42E,H42F} of C42A, {H24D,H24E,H24F} of C24A, {H27D,H27E,H27F} of
  C27A, {H36D,H36E,H36F} of C36B, {H37D,H37E,H37F} of C37B, {H39D,H39E,H39F} of
  C39B, {H37A,H37B,H37C} of C37A, {H40A,H40B,H40C} of C40A, {H39A,H39B,H39C} of
  C39A, {H49A,H49B,H49C} of C49A, {H36A,H36B,H36C} of C36A, {H42A,H42B,H42C} of
  C42B, {H23A,H23B,H23C} of C23B, {H45A,H45B,H45C} of C45B, {H25A,H25B,H25C} of
  C25B, {H24A,H24B,H24C} of C24B, {H48A,H48B,H48C} of C48A, {H46A,H46B,H46C} of
  C46B, {H26A,H26B,H26C} of C26B, {H27A,H27B,H27C} of C27B, {H0AA,H0AB,H0AC} of
  C0AA, {H51A,H51B,H51C} of C51B, {H20A,H20B,H20C} of C20, {H21A,H21B,H21C} of
  C21, {H18A,H18B,H18C} of C18, {H43A,H43B,H43C} of C43, {H19A,H19B,H19C} of
  C19, {H22A,H22B,H22C} of C22, {H1AA,H1AB,H1AC} of C1AA
2. Restrained distances
 O1-C52A \\sim O1-C52B
 with sigma of 0.02
 O1-C55A \\sim O1-C55B
 with sigma of 0.02
 C52A-C53A \\sim C52B-C53B
 with sigma of 0.02
 C53A-C54A \\sim C53B-C54B
 with sigma of 0.02
 C55A-C54A \\sim C55B-C54B
 with sigma of 0.02
 O1-C53A \\sim O1-C53B
 with sigma of 0.04
 O1-C54A \\sim O1-C54B
 with sigma of 0.04
 C52A-C54A \\sim C52B-C54B
 with sigma of 0.04
 C53A-C55A \\sim C53B-C55B
 with sigma of 0.04
3. Rigid bond restraints
 Si3A, C38A, C39A, C40A, Si3B, C35B, C36B, C37B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, C52B, C53B, C54B, C55B, C52A, C53A, C54A, C55A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si3B, C38B, C39B, C40B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14A, C14B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13A, C14A, C15, C16, C11A, C12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C13A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Si3A \\sim C38A \\sim C39A \\sim C40A \\sim Si3B \\sim C35B \\sim C36B \\sim
C37B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O1 \\sim C52B \\sim C53B \\sim C54B \\sim C55B \\sim C52A \\sim C53A \\sim C54A
\\sim C55A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Si3B \\sim C38B \\sim C39B \\sim C40B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C14A \\sim C14B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C13A \\sim C14A \\sim C15 \\sim C16 \\sim C12A \\sim C11A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C14A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C52A, C53A, C54A, C55A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H8B(0.5) H8A(0.5) H15A(0.5) H15B(0.5) H15(0.5) H16A(0.5) H16B(0.5)
 H16(0.5) H41(0.5) H41A(0.5) Si2B(0.5) Si3A(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5)
 H1AC(0.5) C9A(0.5) H9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5) C12A(0.5) H12A(0.5)
 C13A(0.5) H13A(0.5) C14A(0.5) H14A(0.5) C22B(0.5) C23B(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5) C24B(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25B(0.5)
 H25A(0.5) H25B(0.5) H25C(0.5) C26B(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
 C27B(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C35A(0.5) H35A(0.5) C36A(0.5)
 H36A(0.5) H36B(0.5) H36C(0.5) C37A(0.5) H37A(0.5) H37B(0.5) H37C(0.5)
 C38A(0.5) H38A(0.5) C39A(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C40A(0.5)
 H40A(0.5) H40B(0.5) H40C(0.5) C42B(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
 C44B(0.5) H44B(0.5) C45B(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C46B(0.5)
 H46A(0.5) H46B(0.5) H46C(0.5) C47A(0.5) H47A(0.5) C48A(0.5) H48A(0.5)
 H48B(0.5) H48C(0.5) C49A(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C50B(0.5)
 H50B(0.5) C51B(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C52B(0.5) H52A(0.5)
 H52B(0.5) C53B(0.5) H53A(0.5) H53B(0.5) C54B(0.5) H54A(0.5) H54B(0.5)
 C55B(0.5) H55A(0.5) H55B(0.5) Si2A(0.5) Si3B(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) H0AC(0.5) C9B(0.5) H9B(0.5) C10B(0.5) H10B(0.5) C11B(0.5) C12B(0.5)
 H12B(0.5) C13B(0.5) H13B(0.5) C14B(0.5) H14B(0.5) C22A(0.5) C23A(0.5)
 H23D(0.5) H23E(0.5) H23F(0.5) C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
 C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5) C26A(0.5) H26D(0.5) H26E(0.5)
 H26F(0.5) C27A(0.5) H27D(0.5) H27E(0.5) H27F(0.5) C35B(0.5) H35B(0.5)
 C36B(0.5) H36D(0.5) H36E(0.5) H36F(0.5) C37B(0.5) H37D(0.5) H37E(0.5)
 H37F(0.5) C38B(0.5) H38B(0.5) C39B(0.5) H39D(0.5) H39E(0.5) H39F(0.5)
 C40B(0.5) H40D(0.5) H40E(0.5) H40F(0.5) C42A(0.5) H42D(0.5) H42E(0.5)
 H42F(0.5) C44A(0.5) H44A(0.5) C45A(0.5) H45D(0.5) H45E(0.5) H45F(0.5)
 C46A(0.5) H46D(0.5) H46E(0.5) H46F(0.5) C47B(0.5) H47B(0.5) C48B(0.5)
 H48D(0.5) H48E(0.5) H48F(0.5) C49B(0.5) H49D(0.5) H49E(0.5) H49F(0.5)
 C50A(0.5) H50A(0.5) C51A(0.5) H51D(0.5) H51E(0.5) H51F(0.5) C52A(0.5)
 H52C(0.5) H52D(0.5) C53A(0.5) H53C(0.5) H53D(0.5) C54A(0.5) H54C(0.5)
 H54D(0.5) C55A(0.5) H55C(0.5) H55D(0.5)
7.a Ternary CH refined with riding coordinates:
 C41(H41), C41(H41A), C35A(H35A), C38A(H38A), C44B(H44B), C47A(H47A),
 C50B(H50B), C35B(H35B), C38B(H38B), C44A(H44A), C47B(H47B), C50A(H50A)
7.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C52B(H52A,H52B), C53B(H53A,H53B), C54B(H54A,
 H54B), C55B(H55A,H55B), C52A(H52C,H52D), C53A(H53C,H53D), C54A(H54C,H54D),
 C55A(H55C,H55D)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8B), C8(H8A), C15(H15), C16(H16), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C9A(H9A), C10A(H10A), C12A(H12A),
 C13A(H13A), C14A(H14A), C9B(H9B), C10B(H10B), C12B(H12B), C13B(H13B),
 C14B(H14B)
7.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C43(H43A,H43B,H43C), C1AA(H1AA,H1AB,H1AC),
 C23B(H23A,H23B,H23C), C24B(H24A,H24B,H24C), C25B(H25A,H25B,H25C), C26B(H26A,
 H26B,H26C), C27B(H27A,H27B,H27C), C36A(H36A,H36B,H36C), C37A(H37A,H37B,H37C),
 C39A(H39A,H39B,H39C), C40A(H40A,H40B,H40C), C42B(H42A,H42B,H42C), C45B(H45A,
 H45B,H45C), C46B(H46A,H46B,H46C), C48A(H48A,H48B,H48C), C49A(H49A,H49B,H49C),
 C51B(H51A,H51B,H51C), C0AA(H0AA,H0AB,H0AC), C23A(H23D,H23E,H23F), C24A(H24D,
 H24E,H24F), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F),
 C36B(H36D,H36E,H36F), C37B(H37D,H37E,H37F), C39B(H39D,H39E,H39F), C40B(H40D,
 H40E,H40F), C42A(H42D,H42E,H42F), C45A(H45D,H45E,H45F), C46A(H46D,H46E,H46F),
 C48B(H48D,H48E,H48F), C49B(H49D,H49E,H49F), C51A(H51D,H51E,H51F)
;
_shelx_res_checksum              8301
_shelx_hkl_checksum              15619
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'