The effect of substituents on the P-P and PC bond properties in phosphanylphosphaalkenes.
Ziółkowska, Aleksandra; Błaszkiewicz, Wiktoria; Kruczyński, Tomasz; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8041–8044; doi:10.1039/d5dt00692a

data_7718563
_publ_section_title
;
 The effect of substituents on the P-P and P&#xe001;C bond properties in
 phosphanylphosphaalkenes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8041
_journal_page_last               8044
_journal_paper_doi               10.1039/d5dt00692a
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C27 H52 Li N O3 P2 Si'
_chemical_formula_sum            'C27 H52 Li N O3 P2 Si'
_chemical_formula_weight         535.66
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2025-03-10T12:44:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2025-03-20 deposited with the CCDC.	2025-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.930(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6328(7)
_cell_length_b                   18.6610(6)
_cell_length_c                   20.7350(10)
_cell_measurement_reflns_used    24307
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      2.18
_cell_measurement_wavelength     0.71073
_cell_volume                     6435.8(5)
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      ' 215 frames, detector distance = 40 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30597
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.93
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_min         2.183
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.35
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.06(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1214
_refine_ls_number_reflns         19705
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.891
_reflns_Friedel_fraction_max     0.863
_reflns_number_gt                15297
_reflns_number_total             19705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00692a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7718563--7718565.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7718563
_shelx_res_checksum              70093
_shelx_hkl_checksum              72071