#------------------------------------------------------------------------------
#$Date: 2021-10-06 18:32:35 +0300 (Wed, 06 Oct 2021) $
#$Revision: 269706 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/81/7708153.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7708153
loop_
_publ_author_name
'Guschlbauer, Jannick'
'Vollgraff, Tobias'
'Xie, Xiulan'
'Fetoh, Ahmed'
'Sundermeyer, Jörg'
_publ_section_title
;
 Heavy silylchalcogenido lanthanates synthesis
 Ph₄P[Cp₃La-ESiMe₃] (E = S, Se, and Te)
 via fluoride-induced demethylation of dimethylcarbonate to
 Ph₄P[OCO₂Me] 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, ω 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/[σ²(Fo²)+(0.1033P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.35771(6) 0.79893(5) 0.66710(4) 0.02568(18) Uani 1 1 d . . . . .
O1 O 0.8126(3) 0.29485(17) 0.75692(16) 0.0512(5) Uani 1 1 d . . . . .
C1 C 0.0325(3) 0.8365(2) 0.6813(2) 0.0369(5) Uani 1 1 d . . . . .
H1A H 0.071228 0.815935 0.749398 0.055 Uiso 1 1 calc R U . . .
H1B H -0.069545 0.781696 0.641806 0.055 Uiso 1 1 calc R U . . .
H1C H 0.006848 0.918228 0.696152 0.055 Uiso 1 1 calc R U . . .
N1 N 0.1682(2) 0.82667(16) 0.61513(15) 0.0293(4) Uani 1 1 d . . . . .
N2 N 0.4716(2) 0.77130(16) 0.56894(15) 0.0286(4) Uani 1 1 d . . . . .
P2 P 0.37786(6) 0.58936(5) 0.78016(4) 0.02470(18) Uani 1 1 d . . . . .
O2 O 0.8625(3) 0.10262(16) 0.72944(15) 0.0491(5) Uani 1 1 d . . . . .
C2 C 0.1358(3) 0.8733(2) 0.5166(2) 0.0338(5) Uani 1 1 d . . . . .
H2A H 0.137386 0.959624 0.537832 0.051 Uiso 1 1 calc R U . . .
H2B H 0.024956 0.835319 0.473504 0.051 Uiso 1 1 calc R U . . .
H2C H 0.223902 0.855447 0.473889 0.051 Uiso 1 1 calc R U . . .
O3 O 0.9828(2) 0.24207(16) 0.88655(14) 0.0429(4) Uani 1 1 d . . . . .
C3 C 0.4190(3) 0.6601(2) 0.48057(19) 0.0337(5) Uani 1 1 d . . . . .
H3A H 0.342660 0.603590 0.503304 0.051 Uiso 1 1 calc R U . . .
H3B H 0.519399 0.624505 0.464522 0.051 Uiso 1 1 calc R U . . .
H3C H 0.360640 0.679450 0.415971 0.051 Uiso 1 1 calc R U . . .
N3 N 0.4555(2) 0.92058(16) 0.76092(16) 0.0310(4) Uani 1 1 d . . . . .
N4 N 0.2810(2) 0.45650(16) 0.70246(15) 0.0274(4) Uani 1 1 d . . . . .
C4 C 0.5842(3) 0.8653(2) 0.5408(2) 0.0333(5) Uani 1 1 d . . . . .
H4A H 0.617497 0.934078 0.603001 0.050 Uiso 1 1 calc R U . . .
H4B H 0.523453 0.890011 0.479912 0.050 Uiso 1 1 calc R U . . .
H4C H 0.685446 0.833540 0.521186 0.050 Uiso 1 1 calc R U . . .
N6 N 0.5861(2) 0.58941(16) 0.81161(15) 0.0283(4) Uani 1 1 d . . . . .
C6 C 0.6144(3) 0.9169(2) 0.8354(2) 0.0376(6) Uani 1 1 d . . . . .
H6A H 0.608927 0.959942 0.908688 0.056 Uiso 1 1 calc R U . . .
H6B H 0.711584 0.954504 0.812147 0.056 Uiso 1 1 calc R U . . .
H6C H 0.626959 0.833984 0.834230 0.056 Uiso 1 1 calc R U . . .
N5 N 0.3153(2) 0.60759(16) 0.90061(15) 0.0268(4) Uani 1 1 d . . . . .
C5 C 0.4253(3) 1.0442(2) 0.7562(2) 0.0385(6) Uani 1 1 d . . . . .
H5A H 0.418929 1.090255 0.828330 0.058 Uiso 1 1 calc R U . . .
H5B H 0.318581 1.040330 0.707074 0.058 Uiso 1 1 calc R U . . .
H5C H 0.518486 1.082807 0.730190 0.058 Uiso 1 1 calc R U . . .
C7 C 0.1173(3) 0.4422(2) 0.62570(19) 0.0347(5) Uani 1 1 d . . . . .
H7A H 0.097202 0.519816 0.613205 0.052 Uiso 1 1 calc R U . . .
H7B H 0.024688 0.409978 0.656356 0.052 Uiso 1 1 calc R U . . .
H7C H 0.122852 0.387452 0.557292 0.052 Uiso 1 1 calc R U . . .
N7 N 0.3308(2) 0.68662(16) 0.71654(16) 0.0303(4) Uani 1 1 d . . . . .
C9 C 0.1276(3) 0.5755(2) 0.89584(19) 0.0313(5) Uani 1 1 d . . . . .
H9A H 0.104961 0.584183 0.969052 0.047 Uiso 1 1 calc R U . . .
H9B H 0.090285 0.492989 0.854442 0.047 Uiso 1 1 calc R U . . .
H9C H 0.065808 0.628708 0.860929 0.047 Uiso 1 1 calc R U . . .
C8 C 0.3157(3) 0.3461(2) 0.7377(2) 0.0343(5) Uani 1 1 d . . . . .
H8A H 0.235877 0.328247 0.783509 0.051 Uiso 1 1 calc R U . . .
H8B H 0.431606 0.358537 0.778250 0.051 Uiso 1 1 calc R U . . .
H8C H 0.302259 0.279322 0.674240 0.051 Uiso 1 1 calc R U . . .
C10 C 0.3848(3) 0.7225(2) 0.98183(19) 0.0333(5) Uani 1 1 d . . . . .
H10A H 0.355240 0.718306 1.051490 0.050 Uiso 1 1 calc R U . . .
H10B H 0.336449 0.787838 0.958023 0.050 Uiso 1 1 calc R U . . .
H10C H 0.508152 0.736532 0.989170 0.050 Uiso 1 1 calc R U . . .
C11 C 0.6727(3) 0.5435(2) 0.90259(19) 0.0319(5) Uani 1 1 d . . . . .
H11A H 0.591225 0.526326 0.947643 0.048 Uiso 1 1 calc R U . . .
H11B H 0.766211 0.603752 0.946241 0.048 Uiso 1 1 calc R U . . .
H11C H 0.716984 0.470464 0.872980 0.048 Uiso 1 1 calc R U . . .
C12 C 0.6959(3) 0.6026(2) 0.73176(19) 0.0338(5) Uani 1 1 d . . . . .
H12A H 0.738253 0.527412 0.707010 0.051 Uiso 1 1 calc R U . . .
H12B H 0.791553 0.665770 0.765450 0.051 Uiso 1 1 calc R U . . .
H12C H 0.630100 0.623299 0.670214 0.051 Uiso 1 1 calc R U . . .
C13 C 0.8763(3) 0.2090(2) 0.78048(19) 0.0330(5) Uani 1 1 d . . . . .
C14 C 1.0512(3) 0.1464(2) 0.9260(2) 0.0466(6) Uani 1 1 d . . . . .
H14A H 0.958129 0.085980 0.927482 0.070 Uiso 1 1 calc R U . . .
H14B H 1.117416 0.178412 0.998830 0.070 Uiso 1 1 calc R U . . .
H14C H 1.124197 0.110177 0.878169 0.070 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 P1 N1 108.49(9) . . ?
N7 P1 N3 111.78(10) . . ?
N1 P1 N3 108.13(10) . . ?
N7 P1 N2 110.56(10) . . ?
N1 P1 N2 108.84(9) . . ?
N3 P1 N2 108.96(9) . . ?
C1 N1 C2 114.78(18) . . ?
C1 N1 P1 119.85(15) . . ?
C2 N1 P1 123.53(14) . . ?
C4 N2 C3 113.72(18) . . ?
C4 N2 P1 123.76(16) . . ?
C3 N2 P1 119.19(14) . . ?
N7 P2 N6 113.17(9) . . ?
N7 P2 N4 107.09(10) . . ?
N6 P2 N4 110.83(9) . . ?
N7 P2 N5 114.54(10) . . ?
N6 P2 N5 103.32(9) . . ?
N4 P2 N5 107.81(9) . . ?
C13 O3 C14 116.60(19) . . ?
C6 N3 C5 113.64(18) . . ?
C6 N3 P1 120.86(16) . . ?
C5 N3 P1 123.05(16) . . ?
C7 N4 C8 114.28(17) . . ?
C7 N4 P2 122.55(15) . . ?
C8 N4 P2 118.96(15) . . ?
C12 N6 C11 112.51(16) . . ?
C12 N6 P2 120.11(14) . . ?
C11 N6 P2 125.18(14) . . ?
C10 N5 C9 111.19(17) . . ?
C10 N5 P2 116.52(13) . . ?
C9 N5 P2 115.60(14) . . ?
P2 N7 P1 158.50(12) . . ?
O1 C13 O2 131.3(2) . . ?
O1 C13 O3 112.1(2) . . ?
O2 C13 O3 116.6(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N7 1.5591(17) . ?
P1 N1 1.6363(18) . ?
P1 N3 1.6397(18) . ?
P1 N2 1.6442(18) . ?
O1 C13 1.223(3) . ?
C1 N1 1.463(3) . ?
N1 C2 1.465(3) . ?
N2 C4 1.464(2) . ?
N2 C3 1.465(3) . ?
P2 N7 1.5571(18) . ?
P2 N6 1.6362(16) . ?
P2 N4 1.6452(17) . ?
P2 N5 1.6575(18) . ?
O2 C13 1.226(3) . ?
O3 C13 1.421(3) . ?
O3 C14 1.424(3) . ?
N3 C6 1.463(3) . ?
N3 C5 1.470(3) . ?
N4 C7 1.466(3) . ?
N4 C8 1.468(3) . ?
N6 C12 1.457(3) . ?
N6 C11 1.478(3) . ?
N5 C10 1.466(3) . ?
N5 C9 1.482(2) . ?
