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_7708155
_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+, C18 H24 La Se Si 1-'
_chemical_formula_sum            'C42 H44 La P Se Si'
_chemical_formula_weight         825.70
_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     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                 111.185(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1259(9)
_cell_length_b                   17.0307(9)
_cell_length_c                   17.0151(11)
_cell_measurement_reflns_used    28820
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.78
_cell_measurement_theta_min      3.50
_cell_volume                     3816.8(4)
_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)'
'enCIFer (F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler, J. Appl. Cryst. 2004, 37, 335-338.)'
;
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution
'SHELXT (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8.)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35700
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         3.502
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    10.633
_exptl_absorpt_correction_T_max  0.0036
_exptl_absorpt_correction_T_min  0.0004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
STOE LANA, absorption correction by scaling of reflection intensities.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0573P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5742
_reflns_number_total             6749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02000e2.cif
_cod_data_source_block           jg360loesen
_cod_depositor_comments
'Adding full bibliography for 7708147--7708155.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7708155
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              87462