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_7710534
_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 Cl2.136 Ga I0.864 P2'
_chemical_formula_sum            'C21 H38 Cl2.13 Ga I0.87 P2'
_chemical_formula_weight         607.63
_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
_audit_creation_date             2022-03-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-04-13 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.781(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9087(6)
_cell_length_b                   29.337(2)
_cell_length_c                   10.4157(8)
_cell_measurement_reflns_used    13910
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.38
_cell_volume                     2719.0(3)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 262 frames, detector distance = 110 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  0.0240
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22538
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.077
_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    2.327
_exptl_absorpt_correction_T_max  0.7083
_exptl_absorpt_correction_T_min  0.3270
_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_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1229
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.078
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5049
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0600P)^2^+5.2746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1245
_reflns_d_resolution_high        0.756
_reflns_d_resolution_low         9.805
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              38
_reflns_limit_k_min              -38
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                4045
_reflns_number_total             5049
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d2dt01575g2.cif
_cod_data_source_block           ks1569_8MesStar
_cod_original_cell_volume        2718.9(3)
_cod_database_code               7710534
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.480
_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
 C16A-C17A
 2.4 with sigma of 0.01
 C17A-C18A
 2.4 with sigma of 0.01
 C15-C16 \\sim C15-C16A
 with sigma of 0.02
 C15-C18 \\sim C15-C16A
 with sigma of 0.02
 C15-C17 \\sim C15-C18A
 with sigma of 0.02
 C17A-C15 \\sim C16A-C15 \\sim C18A-C15 \\sim C17-C15 \\sim C18-C15 \\sim
C16-C15
 with sigma of 0.01
 I1-Ga1 \\sim I2-Ga1
 with sigma of 0.01
 Ga1-Cl2 \\sim Ga1-Cl1 \\sim Ga1-Cl3
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(I1) = Uanis(Cl3)
Uanis(C18) = Uanis(C18A)
Uanis(C17) = Uanis(C16A)
Uanis(C16) = Uanis(C17A)
Uanis(C17) = Uanis(C17A)
Uanis(Cl1) = Uanis(I3)
Uanis(Cl2) = Uanis(I2)
4. Others
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Sof(I1)=1-FVAR(2)
 Sof(Cl3)=FVAR(2)
 Sof(I2)=1-FVAR(3)
 Sof(Cl2)=FVAR(3)
 Sof(I3)=1-FVAR(4)
 Sof(Cl1)=FVAR(4)
5.a Me refined with riding coordinates:
 C18A(H18D,H18E,H18F), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C17(H17A,
 H17B,H17C)
;
_shelx_res_checksum              32502
_shelx_hkl_checksum              48968
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '110.0 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 98.7
_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 56.1
_stoe_evaluation_lana_max_2theta_desired 56.1
_stoe_evaluation_lana_mean_redundancy 3.0
_stoe_evaluation_lana_number_refls_after_or 92211
_stoe_evaluation_lana_number_refls_outliers 9446
_stoe_evaluation_lana_number_refls_total 101657
_stoe_evaluation_lana_number_refls_unique 30677
_stoe_evaluation_lana_number_refls_written 92211
_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 -1
_stoe_evaluation_lana_table
;
2Theta           5.6   11.6   17.6   23.6   29.6   35.6   41.6   47.6   53.6
<Resolution>    6.14   3.37   2.28   1.72   1.38   1.16   1.00   0.88   0.79
N(total)         447   1723   3924   6750  10274  14155  18717  22823  22844
<Redundancy>     2.7    2.8    2.9    2.9    3.0    3.0    3.0    3.1    3.0
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0  100.0   94.7
<I/sigma>      102.7   58.3   22.3   16.4    6.3    3.4    1.7    0.7    0.2
R(int)         0.015  0.019  0.025  0.029  0.062  0.105  0.187  0.378  0.614
;
_stoe_measurement_identifier     ks1572
_stoe_measurement_max_exposure_per_frame '1200.0 s'
_stoe_measurement_mean_exposure_per_frame '1200.0 s'
_stoe_measurement_min_exposure_per_frame '1200.0 s'
_stoe_measurement_total_exposure_time '109.7 h'
_stoe_measurement_total_frame_number 329
_stoe_measurement_total_run_number 2
_stoe_measurement_tube_power     '1.5 kW'