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_1565669
_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         'C54 H88 Er Pb Si4, 2(C8 H16 Li0.5 O4)'
_chemical_formula_sum            'C73.5 H124 Er Li O8 Pb Si4'
_chemical_formula_weight         1629.47
_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
_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                90.114(7)
_cell_angle_beta                 99.276(5)
_cell_angle_gamma                109.783(8)
_cell_formula_units_Z            2
_cell_length_a                   13.1318(10)
_cell_length_b                   13.3996(16)
_cell_length_c                   24.0543(14)
_cell_measurement_reflns_used    70235
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      1.88
_cell_volume                     3923.4(6)
_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                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_details
;
 1290 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  StadiVari
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46121
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.336
_diffrn_reflns_theta_min         1.878
_diffrn_source                   'Mo GeniX 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.315
_exptl_absorpt_correction_T_max  0.7611
_exptl_absorpt_correction_T_min  0.3924
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1676
_exptl_crystal_recrystallization_method
'The material was recrystallised from hot toluene by cooling to room temperature'
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         19762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.6012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16136
_reflns_number_total             19762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03805b2.cif
_cod_data_source_block           lmmxf229_12-c-4
_cod_depositor_comments
'Adding full bibliography for 1565662--1565670.cif.'
_cod_original_formula_sum        'C73.50 H124 Er Li O8 Pb Si4'
_cod_database_code               1565669
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.553
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O2B(0.5) O6A(0.5) O4B(0.5) H68A(0.5) H68B(0.5) H68C(0.5) H68D(0.5)
 H57C(0.5) H57D(0.5) H57A(0.5) H57B(0.5) H61C(0.5) H61D(0.5) H61A(0.5)
 H61B(0.5) O8A(0.5) H70A(0.5) H70B(0.5) H70C(0.5) H70D(0.5) O2A(0.5) O4A(0.5)
 H55A(0.5) H55B(0.5) H55C(0.5) H55D(0.5) O1A(0.5) O1B(0.5) O3A(0.5) H66C(0.5)
 H66D(0.5) H66A(0.5) H66B(0.5) O6B(0.5) O5A(0.5) O8B(0.5) O5B(0.5) O7A(0.5)
 C65A(0.5) H65A(0.5) H65B(0.5) C67B(0.5) H67A(0.5) H67B(0.5) C69B(0.5)
 H69A(0.5) H69B(0.5) C63A(0.5) H63A(0.5) H63B(0.5) C69A(0.5) H69C(0.5)
 H69D(0.5) C63B(0.5) H63C(0.5) H63D(0.5) O7B(0.5) C67A(0.5) H67C(0.5) H67D(0.5)
 C65B(0.5) H65C(0.5) H65D(0.5) H64C(0.5) H64D(0.5) H64A(0.5) H64B(0.5) O3B(0.5)
 C56A(0.5) H56A(0.5) H56B(0.5) C56B(0.5) H56C(0.5) H56D(0.5) C58A(0.5)
 H58A(0.5) H58B(0.5) C60B(0.5) H60A(0.5) H60B(0.5) C60A(0.5) H60C(0.5)
 H60D(0.5) C58B(0.5) H58C(0.5) H58D(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
 H59D(0.5) C62A(0.5) H62A(0.5) H62B(0.5) C62B(0.5) H62C(0.5) H62D(0.5)
3.a Ternary CH refined with riding coordinates:
 C43(H43), C52(H52), C37(H37), C40(H40), C46(H46), C49(H49)
3.b Secondary CH2 refined with riding coordinates:
 C68A(H68A,H68B), C68A(H68C,H68D), C57(H57C,H57D), C57(H57A,H57B), C61(H61C,
 H61D), C61(H61A,H61B), C70A(H70A,H70B), C70A(H70C,H70D), C55(H55A,H55B),
 C55(H55C,H55D), C66A(H66C,H66D), C66A(H66A,H66B), C65A(H65A,H65B), C67B(H67A,
 H67B), C69B(H69A,H69B), C63A(H63A,H63B), C69A(H69C,H69D), C63B(H63C,H63D),
 C67A(H67C,H67D), C65B(H65C,H65D), C64A(H64C,H64D), C64A(H64A,H64B), C56A(H56A,
 H56B), C56B(H56C,H56D), C58A(H58A,H58B), C60B(H60A,H60B), C60A(H60C,H60D),
 C58B(H58C,H58D), C59(H59A,H59B), C59(H59C,H59D), C62A(H62A,H62B), C62B(H62C,
 H62D)
3.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C33(H33), C32(H32), C30(H30), C6(H6), C9(H9), C31(H31), C10(H10),
 C8(H8), C16(H16), C15(H15), C13(H13), C7(H7), C14(H14), C12(H12), C35(H35)
3.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C39(H39A,H39B,
 H39C), C38(H38A,H38B,H38C), C27(H27A,H27B,H27C), C53(H53A,H53B,H53C), C44(H44A,
 H44B,H44C), C42(H42A,H42B,H42C), C51(H51A,H51B,H51C), C19(H19A,H19B,H19C),
 C28(H28A,H28B,H28C), C41(H41A,H41B,H41C), C50(H50A,H50B,H50C), C48(H48A,H48B,
 H48C), C54(H54A,H54B,H54C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C18(H18A,
 H18B,H18C), C24(H24A,H24B,H24C), C47(H47A,H47B,H47C), C45(H45A,H45B,H45C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 52 electrons were 
found in a volume of 165\%A^3 in 1 void. 
This is consistent with the presence of 
0.5[C7H8] per formula unit 
which account for 50.0 electrons.
;
_smtbx_masks_void_probe_radius   1.7
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35079
_shelx_hkl_checksum              57258
_shelx_fab_checksum              71401
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in mineral oil'
_olex2_submission_special_instructions 'No special instructions were received'