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_7708153
_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         'C12 H36 N7 P2 1+, C2 H3 O3 1-'
_chemical_formula_sum            'C14 H39 N7 O3 P2'
_chemical_formula_weight         415.46
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-31 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                103.005(2)
_cell_angle_beta                 98.958(2)
_cell_angle_gamma                96.125(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9237(2)
_cell_length_b                   11.4184(4)
_cell_length_c                   12.7068(4)
_cell_measurement_reflns_used    16662
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.02
_cell_measurement_theta_min      3.63
_cell_volume                     1094.44(6)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18979
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.482
_diffrn_reflns_theta_max         66.482
_diffrn_reflns_theta_min         4.017
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    2.041
_exptl_absorpt_correction_T_max  0.5688
_exptl_absorpt_correction_T_min  0.0930
_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    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0478
_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^)+(0.1033P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3160
_reflns_number_total             3829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02000e2.cif
_cod_data_source_block           tvd136loesen
_cod_depositor_comments
'Adding full bibliography for 7708147--7708155.cif.'
_cod_database_code               7708153
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              31152