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_1565668
_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 H96 Ce Li O Pb Si4'
_chemical_formula_sum            'C58 H96 Ce Li O Pb Si4'
_chemical_formula_weight         1275.95
_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             2021-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-02 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.5760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4211(2)
_cell_length_b                   13.6559(2)
_cell_length_c                   16.7671(3)
_cell_measurement_reflns_used    70004
_cell_measurement_temperature    150
_cell_measurement_theta_max      64.36
_cell_measurement_theta_min      2.31
_cell_volume                     3046.20(8)
_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      150.0
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
 2149 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36517
_diffrn_reflns_point_group_measured_fraction_full 0.742
_diffrn_reflns_point_group_measured_fraction_max 0.698
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         64.042
_diffrn_reflns_theta_min         2.313
_exptl_absorpt_coefficient_mu    8.124
_exptl_absorpt_correction_T_max  0.0877
_exptl_absorpt_correction_T_min  0.0106
_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    1.391
_exptl_crystal_description       needle
_exptl_crystal_F_000             1302
_exptl_crystal_size_max          0.871
_exptl_crystal_size_mid          0.549
_exptl_crystal_size_min          0.324
_refine_diff_density_max         0.910
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 2699 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         10731
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+6.5157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.363
_reflns_Friedel_fraction_full    0.461
_reflns_Friedel_fraction_max     0.388
_reflns_number_gt                10291
_reflns_number_total             10731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03805b2.cif
_cod_data_source_block           xf221a
_cod_depositor_comments
'Adding full bibliography for 1565662--1565670.cif.'
_cod_database_code               1565668
_shelx_shelxl_version_number     2018/3
_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 C(H,H,H) groups
2. Rigid bond restraints
 C52B, C53B, C54B, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C52B \\sim C53B \\sim C54B \\sim C52A \\sim C53A \\sim C54A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C54B \\sim C52B \\sim C54A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C54B \\sim C52B \\sim C53B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Fixed Sof: C52B(0.5) H52B(0.5) C53B(0.5) H53A(0.5) H53B(0.5) H53C(0.5)
 C54B(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C52A(0.5) H52A(0.5) C53A(0.5)
 H53D(0.5) H53E(0.5) H53F(0.5) C54A(0.5) H54D(0.5) H54E(0.5) H54F(0.5)
5.a Ternary CH refined with riding coordinates:
 C37(H37), C40(H40), C43(H43), C46(H46), C49(H49), C52B(H52B), C52A(H52A)
5.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36)
5.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), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C53B(H53A,H53B,H53C), C54B(H54A,H54B,H54C),
 C53A(H53D,H53E,H53F), C54A(H54D,H54E,H54F)
;
_shelx_res_checksum              75775
_shelx_hkl_checksum              40148
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'