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_1565667
_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, C16 H38.8 Li O4'
_chemical_formula_sum            'C70 H126.8 Er Li O4 Pb Si4'
_chemical_formula_weight         1526.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-29
_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                 113.880(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0069(7)
_cell_length_b                   16.3287(4)
_cell_length_c                   22.8084(7)
_cell_measurement_reflns_used    43054
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.83
_cell_measurement_theta_min      1.58
_cell_volume                     7494.4(4)
_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 0.989
_diffrn_measured_fraction_theta_max 0.836
_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  0.0557
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41204
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.184
_diffrn_reflns_theta_min         1.584
_exptl_absorpt_coefficient_mu    3.462
_exptl_absorpt_correction_T_max  0.5480
_exptl_absorpt_correction_T_min  0.3077
_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    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             3151
_exptl_crystal_size_max          0.777
_exptl_crystal_size_mid          0.603
_exptl_crystal_size_min          0.404
_refine_diff_density_max         2.076
_refine_diff_density_min         -2.910
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         18594
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0726P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14645
_reflns_number_total             18594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03805b2.cif
_cod_data_source_block           lmm150
_cod_depositor_comments
'Adding full bibliography for 1565662--1565670.cif.'
_cod_original_formula_sum        'C70 H126.80 Er Li O4 Pb Si4'
_cod_database_code               1565667
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.335
_shelx_estimated_absorpt_t_min   0.174
_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
 C67, C68, C73, C74
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C65, C66, C64, O3, C63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C66 \\sim O3 \\sim C65 \\sim C63 \\sim C64: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O4, C67, C68, C73, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C67(0.4) H67A(0.4) H67B(0.4) C68(0.4) H68A(0.4) H68B(0.4)
 H68C(0.4) C73(0.4) H73A(0.4) H73B(0.4) C74(0.4) H74A(0.4) H74B(0.4) H74C(0.4)
 C69(0.6) H69A(0.6) H69B(0.6) C70(0.6) H70A(0.6) H70B(0.6) C71(0.6) H71A(0.6)
 H71B(0.6) C72(0.6) H72A(0.6) H72B(0.6)
6.a Ternary CH refined with riding coordinates:
 C37(H37), C40(H40), C43(H43), C46(H46), C49(H49), C52(H52)
6.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B), C63(H63A,
 H63B), C65(H65A,H65B), C67(H67A,H67B), C73(H73A,H73B), C69(H69A,H69B),
 C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C6(H6), C7(H7), C8(H8),
 C9(H9), C10(H10), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36)
6.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), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C62(H62A,H62B,
 H62C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C74(H74A,
 H74B,H74C)
;
_shelx_res_checksum              26291
_shelx_hkl_checksum              40241
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'