Modulating the reactivity of phosphanylidenephosphoranes towards water with Lewis acids
Dankert, Fabian; Fischer, Malte; Hering-Junghans, Christian; Dalton Transactions  (2022) –; doi:10.1039/D2DT01575G

data_7710544
_publ_section_title
;
 Modulating the reactivity of phosphanylidenephosphoranes towards water
 with Lewis acids
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01575G
_journal_year                    2022
_chemical_formula_moiety         'C21 H38 Cl3 Ga P2'
_chemical_formula_sum            'C21 H38 Cl3 Ga P2'
_chemical_formula_weight         528.52
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-04-13 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.085(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8319(9)
_cell_length_b                   29.260(2)
_cell_length_c                   10.3380(11)
_cell_measurement_reflns_used    8328
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.08
_cell_measurement_theta_min      1.98
_cell_volume                     2664.8(4)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
 144 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15355
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.094
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.500
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_T_max  0.7230
_exptl_absorpt_correction_T_min  0.5648
_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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5757
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0536P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0889
_reflns_d_resolution_high        0.727
_reflns_d_resolution_low         9.725
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              40
_reflns_limit_k_min              -29
_reflns_limit_l_max              11
_reflns_limit_l_min              -14
_reflns_number_gt                4027
_reflns_number_total             5757
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d2dt01575g2.cif
_cod_data_source_block           ks1564_cmpd_6MesStar
_cod_original_cell_volume        2664.8(5)
_cod_database_code               7710544
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-C11 \\sim C12-C11 \\sim C23-C11 \\sim C13-C11 \\sim C24-C11 \\sim C14-C11
 with sigma of 0.02
 C12-C11 \\sim C22-C11 \\sim C14-C11 \\sim C24-C11 \\sim C13-C11 \\sim C23-C11
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C23)
4. Others
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
5.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C9(H9A,H9B,H9C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C18(H18A,
 H18B,H18C), C21(H21A,H21B,H21C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              49062
_shelx_hkl_checksum              35694
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '100.0 mm'
_stoe_detector_pixelsize_x       '0.150 mm'
_stoe_detector_pixelsize_y       '0.150 mm'
_stoe_detector_size_x            '34.0 cm'
_stoe_detector_size_y            '34.0 cm'
_stoe_evaluation_integration_a   12.0
_stoe_evaluation_integration_b   0.0
_stoe_evaluation_integration_ems 0.012
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 97.4
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 58.6
_stoe_evaluation_lana_max_2theta_desired 58.6
_stoe_evaluation_lana_mean_redundancy 2.6
_stoe_evaluation_lana_number_refls_after_or 19055
_stoe_evaluation_lana_number_refls_outliers 1301
_stoe_evaluation_lana_number_refls_total 20356
_stoe_evaluation_lana_number_refls_unique 7247
_stoe_evaluation_lana_number_refls_written 19055
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta           6.5   12.7   18.9   25.1   31.3   37.5   43.7   49.9   56.1
<Resolution>    5.33   3.10   2.13   1.62   1.31   1.10   0.95   0.84   0.76
N(total)          96    389    845   1399   2173   2921   3681   4481   4371
<Redundancy>     2.9    3.0    2.8    2.7    2.7    2.6    2.6    2.6    2.6
Complet. [%%]    75.0   88.7   95.5   97.0   99.3  100.0  100.0  100.0   92.5
<I/sigma>      273.6  131.6   75.2   47.2   19.5   13.0    6.6    2.9    1.4
R(int)         0.006  0.009  0.012  0.014  0.023  0.029  0.050  0.098  0.184
;
_stoe_measurement_identifier     ks1564
_stoe_measurement_max_exposure_per_frame '480.0 s'
_stoe_measurement_mean_exposure_per_frame '480.0 s'
_stoe_measurement_min_exposure_per_frame '480.0 s'
_stoe_measurement_total_exposure_time '19.2 h'
_stoe_measurement_total_frame_number 144
_stoe_measurement_total_run_number 1
_stoe_measurement_tube_power     '1.5 kW'