#------------------------------------------------------------------------------
#$Date: 2025-08-21 22:04:39 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301851 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/21/7052180.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_7052180
loop_
_publ_author_name
'Moores, Audrey'
'Cantat, Thibault'
'Ricard, Louis'
'Mézailles, Nicolas'
'Le Floch, Pascal'
_publ_section_title
;
 Experimental and theoretical study of phosphinine sulfides
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1493
_journal_paper_doi               10.1039/b702851b
_journal_volume                  31
_journal_year                    2007
_chemical_formula_moiety         'C23 H29 P Si2'
_chemical_formula_sum            'C23 H29 P Si2'
_chemical_formula_weight         392.61
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.022(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.081(1)
_cell_length_b                   17.513(1)
_cell_length_c                   12.328(1)
_cell_measurement_reflns_used    251
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.0
_cell_volume                     2302.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11250
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.9644
_exptl_absorpt_correction_T_min  0.9558
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         6684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0620P)²+0.1790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                5111
_reflns_number_total             6684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702851b.txt
_cod_data_source_block           psi2ph2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P21/n '
_cod_database_code               7052180
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.55850(3) 0.169090(18) 0.12275(3) 0.02654(10) Uani 1 1 d . . .
Si1 Si 0.30235(3) 0.21143(2) 0.10274(3) 0.02626(10) Uani 1 1 d . . .
Si2 Si 0.83034(4) 0.14467(2) 0.17062(4) 0.02722(10) Uani 1 1 d . . .
C1 C 0.46066(12) 0.24246(7) 0.12216(12) 0.0238(3) Uani 1 1 d . . .
C2 C 0.50187(12) 0.31894(7) 0.13996(12) 0.0243(3) Uani 1 1 d . . .
C3 C 0.61893(13) 0.34103(7) 0.15444(12) 0.0262(3) Uani 1 1 d . . .
H3 H 0.6376 0.3941 0.1643 0.031 Uiso 1 1 calc R . .
C4 C 0.71143(12) 0.29255(7) 0.15580(11) 0.0241(3) Uani 1 1 d . . .
C5 C 0.69750(12) 0.21254(7) 0.14485(11) 0.0244(3) Uani 1 1 d . . .
C6 C 0.28534(17) 0.10609(9) 0.07787(18) 0.0475(4) Uani 1 1 d . . .
H6A H 0.2037 0.0898 0.0686 0.071 Uiso 1 1 calc R . .
H6B H 0.3523 0.0800 0.1486 0.071 Uiso 1 1 calc R . .
H6C H 0.2910 0.0931 0.0033 0.071 Uiso 1 1 calc R . .
C7 C 0.28730(16) 0.23162(10) 0.24348(14) 0.0433(4) Uani 1 1 d . . .
H7A H 0.2835 0.2869 0.2533 0.065 Uiso 1 1 calc R . .
H7B H 0.3600 0.2106 0.3154 0.065 Uiso 1 1 calc R . .
H7C H 0.2105 0.2079 0.2359 0.065 Uiso 1 1 calc R . .
C8 C 0.17180(15) 0.25745(10) -0.03317(16) 0.0457(4) Uani 1 1 d . . .
H8A H 0.0917 0.2360 -0.0459 0.068 Uiso 1 1 calc R . .
H8B H 0.1823 0.2481 -0.1062 0.068 Uiso 1 1 calc R . .
H8C H 0.1726 0.3126 -0.0191 0.068 Uiso 1 1 calc R . .
C9 C 0.42193(13) 0.38379(7) 0.14280(13) 0.0267(3) Uani 1 1 d . . .
C10 C 0.42929(15) 0.40953(8) 0.25178(14) 0.0359(3) Uani 1 1 d . . .
H10 H 0.4812 0.3834 0.3261 0.043 Uiso 1 1 calc R . .
C11 C 0.36172(15) 0.47314(9) 0.25408(16) 0.0408(4) Uani 1 1 d . . .
H11 H 0.3678 0.4902 0.3298 0.049 Uiso 1 1 calc R . .
C12 C 0.28619(16) 0.51150(8) 0.14731(18) 0.0423(4) Uani 1 1 d . . .
H12 H 0.2399 0.5549 0.1490 0.051 Uiso 1 1 calc R . .
C13 C 0.2782(2) 0.48686(11) 0.03919(19) 0.0584(5) Uani 1 1 d . . .
H13 H 0.2262 0.5132 -0.0349 0.070 Uiso 1 1 calc R . .
C14 C 0.34592(19) 0.42322(10) 0.03654(16) 0.0512(5) Uani 1 1 d . . .
H14 H 0.3397 0.4067 -0.0395 0.061 Uiso 1 1 calc R . .
C15 C 0.82741(12) 0.33137(7) 0.17058(12) 0.0259(3) Uani 1 1 d . . .
C16 C 0.86401(14) 0.32791(8) 0.07947(15) 0.0336(3) Uani 1 1 d . . .
H16 H 0.8157 0.2993 0.0068 0.040 Uiso 1 1 calc R . .
C17 C 0.97095(17) 0.36610(9) 0.09419(18) 0.0457(4) Uani 1 1 d . . .
H17 H 0.9959 0.3633 0.0318 0.055 Uiso 1 1 calc R . .
C18 C 1.04098(16) 0.40805(10) 0.1989(2) 0.0530(5) Uani 1 1 d . . .
H18 H 1.1145 0.4337 0.2090 0.064 Uiso 1 1 calc R . .
C19 C 1.00446(16) 0.41277(10) 0.28908(18) 0.0489(4) Uani 1 1 d . . .
H19 H 1.0525 0.4421 0.3610 0.059 Uiso 1 1 calc R . .
C20 C 0.89815(14) 0.37502(8) 0.27528(14) 0.0360(3) Uani 1 1 d . . .
H20 H 0.8731 0.3788 0.3375 0.043 Uiso 1 1 calc R . .
C21 C 0.78400(16) 0.04667(8) 0.19502(15) 0.0388(4) Uani 1 1 d . . .
H21A H 0.7099 0.0299 0.1203 0.058 Uiso 1 1 calc R . .
H21B H 0.7645 0.0477 0.2637 0.058 Uiso 1 1 calc R . .
H21C H 0.8533 0.0111 0.2138 0.058 Uiso 1 1 calc R . .
C22 C 0.86237(16) 0.13613(9) 0.03662(15) 0.0396(4) Uani 1 1 d . . .
H22A H 0.9114 0.1803 0.0349 0.059 Uiso 1 1 calc R . .
H22B H 0.7828 0.1345 -0.0397 0.059 Uiso 1 1 calc R . .
H22C H 0.9097 0.0892 0.0444 0.059 Uiso 1 1 calc R . .
C23 C 0.97628(14) 0.17412(9) 0.31036(14) 0.0374(3) Uani 1 1 d . . .
H23A H 1.0349 0.1311 0.3397 0.056 Uiso 1 1 calc R . .
H23B H 0.9553 0.1897 0.3748 0.056 Uiso 1 1 calc R . .
H23C H 1.0152 0.2170 0.2899 0.056 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
C1 P1 C5 106.27(6) . . ?
C8 Si1 C7 110.15(8) . . ?
C8 Si1 C6 107.40(8) . . ?
C7 Si1 C6 106.84(8) . . ?
C8 Si1 C1 111.61(7) . . ?
C7 Si1 C1 111.29(7) . . ?
C6 Si1 C1 109.36(7) . . ?
C23 Si2 C22 109.82(8) . . ?
C23 Si2 C21 109.20(7) . . ?
C22 Si2 C21 105.66(7) . . ?
C23 Si2 C5 109.79(6) . . ?
C22 Si2 C5 114.27(6) . . ?
C21 Si2 C5 107.91(6) . . ?
C2 C1 P1 120.69(10) . . ?
C2 C1 Si1 123.68(10) . . ?
P1 C1 Si1 115.58(7) . . ?
C3 C2 C1 123.10(12) . . ?
C3 C2 C9 114.32(11) . . ?
C1 C2 C9 122.57(12) . . ?
C2 C3 C4 126.18(12) . . ?
C3 C4 C5 122.94(12) . . ?
C3 C4 C15 115.16(11) . . ?
C5 C4 C15 121.90(12) . . ?
C4 C5 P1 120.75(10) . . ?
C4 C5 Si2 123.52(10) . . ?
P1 C5 Si2 115.38(7) . . ?
C10 C9 C14 118.06(13) . . ?
C10 C9 C2 121.45(12) . . ?
C14 C9 C2 120.30(13) . . ?
C9 C10 C11 120.81(14) . . ?
C12 C11 C10 120.31(15) . . ?
C13 C12 C11 119.53(14) . . ?
C12 C13 C14 120.33(16) . . ?
C9 C14 C13 120.96(16) . . ?
C16 C15 C20 118.89(13) . . ?
C16 C15 C4 121.33(12) . . ?
C20 C15 C4 119.71(13) . . ?
C15 C16 C17 120.24(15) . . ?
C18 C17 C16 120.23(17) . . ?
C17 C18 C19 119.99(16) . . ?
C18 C19 C20 120.23(16) . . ?
C19 C20 C15 120.41(15) . . ?
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 C1 1.7436(13) . ?
P1 C5 1.7445(14) . ?
Si1 C8 1.8605(16) . ?
Si1 C7 1.8614(16) . ?
Si1 C6 1.8655(16) . ?
Si1 C1 1.8922(14) . ?
Si2 C23 1.8677(16) . ?
Si2 C22 1.8713(16) . ?
Si2 C21 1.8729(15) . ?
Si2 C5 1.9000(13) . ?
C1 C2 1.4097(17) . ?
C2 C3 1.3943(19) . ?
C2 C9 1.5018(18) . ?
C3 C4 1.3973(18) . ?
C4 C5 1.4101(17) . ?
C4 C15 1.4896(18) . ?
C9 C10 1.380(2) . ?
C9 C14 1.381(2) . ?
C10 C11 1.389(2) . ?
C11 C12 1.374(2) . ?
C12 C13 1.361(3) . ?
C13 C14 1.392(2) . ?
C15 C16 1.388(2) . ?
C15 C20 1.3944(19) . ?
C16 C17 1.389(2) . ?
C17 C18 1.377(3) . ?
C18 C19 1.377(3) . ?
C19 C20 1.382(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21141601
2 PubChem 15778253
