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_7708149
_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         'C36 H30 N P2 1+, C2 H3 O3 1-, 0.5(C2 H3 N)'
_chemical_formula_sum            'C39 H34.5 N1.5 O3 P2'
_chemical_formula_weight         634.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 97.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.620(2)
_cell_length_b                   35.750(7)
_cell_length_c                   17.320(3)
_cell_measurement_reflns_used    9109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.1306
_cell_measurement_theta_min      2.2439
_cell_volume                     6522(2)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service v3.0.26'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 Quest (Bruker AXS Inc.)'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            175989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'I\mS Microfocus Source'
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.633
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.232
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         11537
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+5.7788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9648
_reflns_number_total             11537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02000e2.cif
_cod_data_source_block           hq07_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7708147--7708155.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C78 H69 N3 O6 P4'
_cod_original_formula_weight         1268.24
_cod_original_formula_moiety     '2(C36 H30 N P2 1+), 2(C2 H3 O3 1-), C2 H3 N'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        6521(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7708149
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.898
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              96411