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_1565665
_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_formula_moiety         'C58 H96 Er Li O Pb Si4'
_chemical_formula_sum            'C58 H96 Er Li O Pb Si4'
_chemical_formula_weight         1303.09
_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                 97.425(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3164(4)
_cell_length_b                   13.3190(3)
_cell_length_c                   16.7792(6)
_cell_measurement_reflns_used    49746
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.24
_cell_measurement_theta_min      1.96
_cell_volume                     2951.02(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details
;
 716 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  StadiVari
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48486
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.506
_diffrn_reflns_theta_min         1.959
_diffrn_source                   'Mo GeniX 3D HF'
_exptl_absorpt_coefficient_mu    4.378
_exptl_absorpt_correction_T_max  0.5494
_exptl_absorpt_correction_T_min  0.2900
_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    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1322
_exptl_crystal_recrystallization_method
'The material was recrystallised from hot toluene by cooling to room temperature'
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Flack x determined using 5676 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         16698
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.812
_reflns_number_gt                13996
_reflns_number_total             16698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03805b2.cif
_cod_data_source_block           lmm150_toluene
_cod_depositor_comments
'Adding full bibliography for 1565662--1565670.cif.'
_cod_database_code               1565665
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.290
_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.a Ternary CH refined with riding coordinates:
 C43(H43), C40(H40), C37(H37), C49(H49), C52(H52), C46(H46)
2.b Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C7(H7), C6(H6), C31(H31), C36(H36), C16(H16), C13(H13), C8(H8),
 C9(H9), C35(H35), C33(H33), C15(H15), C12(H12), C10(H10), C14(H14), C30(H30)
2.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C19(H19A,H19B,
 H19C), C38(H38A,H38B,H38C), C28(H28A,H28B,H28C), C44(H44A,H44B,H44C), C42(H42A,
 H42B,H42C), C45(H45A,H45B,H45C), C24(H24A,H24B,H24C), C18(H18A,H18B,H18C),
 C50(H50A,H50B,H50C), C25(H25A,H25B,H25C), C20(H20A,H20B,H20C), C48(H48A,H48B,
 H48C), C51(H51A,H51B,H51C), C39(H39A,H39B,H39C), C53(H53A,H53B,H53C), C27(H27A,
 H27B,H27C), C47(H47A,H47B,H47C), C54(H54A,H54B,H54C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              3805
_shelx_hkl_checksum              27224
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'