Heavy silylchalcogenido lanthanates synthesis Ph<sub>4</sub>P[Cp<sub>3</sub>La-ESiMe<sub>3</sub>] (E = S, Se, and Te) <i>via</i> fluoride-induced demethylation of dimethylcarbonate to Ph<sub>4</sub>P[OCO<sub>2</sub>Me] key intermediate.
Guschlbauer, Jannick; Vollgraff, Tobias; Xie, Xiulan; Fetoh, Ahmed; Sundermeyer, Jörg; Dalton transactions (Cambridge, England : 2003) 50 (2021) 13103–13111; doi:10.1039/d1dt02000e

data_7708151
_publ_section_title
;
 Heavy silylchalcogenido lanthanates synthesis
 Ph<sub>4</sub>P[Cp<sub>3</sub>La-ESiMe<sub>3</sub>] (E = S, Se, and Te)
 <i>via</i> fluoride-induced demethylation of dimethylcarbonate to
 Ph<sub>4</sub>P[OCO<sub>2</sub>Me] key intermediate.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13103
_journal_page_last               13111
_journal_paper_doi               10.1039/d1dt02000e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C24 H20 P 1+, C3 H9 Si Te 1-'
_chemical_formula_sum            'C27 H29 P Si Te'
_chemical_formula_weight         540.16
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-05-31 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.136(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5283(2)
_cell_length_b                   10.6121(2)
_cell_length_c                   12.3821(3)
_cell_measurement_reflns_used    23045
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.10
_cell_measurement_theta_min      3.57
_cell_volume                     1252.02(5)
_computing_cell_refinement
; 
X-Area Recipe 1.33.0.0 (STOE, 2015) 
;
_computing_data_collection
; 
X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016) 
;
_computing_data_reduction
; 
X-Area Integrate 1.71.0.0 (STOE, 2016) 
X-Area LANA 1.68.2.0 (STOE, 2016) 
;
_computing_molecular_graphics
'DIAMOND 4 (H. Putz, K. Brandenburg, Crystal Impact GbR, Kreuzherrenstr. 102, 53227 Bonn, Germany)'
_computing_publication_material
'WinGX 2014.1 (L.J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19271
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.487
_diffrn_reflns_theta_max         66.487
_diffrn_reflns_theta_min         3.570
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    10.510
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
STOE LANA, absorption correction by scaling of reflection intensities. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.043
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.051(10)
_refine_ls_extinction_coef       0.0020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0865P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3746
_reflns_number_total             3978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02000e2.cif
_cod_data_source_block           jg354loesen
_cod_depositor_comments
'Adding full bibliography for 7708147--7708155.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7708151
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              51173