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_7710536
_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         'C24 H27 Ga I3 O P'
_chemical_formula_sum            'C24 H27 Ga I3 O P'
_chemical_formula_weight         812.84
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_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   mixed
_atom_sites_solution_primary     dual
_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                107.115(8)
_cell_angle_beta                 104.929(8)
_cell_angle_gamma                99.870(9)
_cell_formula_units_Z            2
_cell_length_a                   10.8322(12)
_cell_length_b                   11.4626(12)
_cell_length_c                   13.0010(14)
_cell_measurement_reflns_used    13937
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.36
_cell_measurement_theta_min      1.67
_cell_volume                     1436.3(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 279 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  0.0124
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14121
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.496
_diffrn_reflns_theta_min         1.734
_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    4.251
_exptl_absorpt_correction_T_max  0.2834
_exptl_absorpt_correction_T_min  0.2259
_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    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_exptl_crystal_size_rad          0.078
_refine_diff_density_max         3.377
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5355
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0450
_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/[\s^2^(Fo^2^)+(0.0736P)^2^+3.2723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1334
_reflns_d_resolution_high        0.728
_reflns_d_resolution_low         11.741
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              15
_reflns_limit_l_min              -17
_reflns_number_gt                4293
_reflns_number_total             5355
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d2dt01575g2.cif
_cod_data_source_block           ks1566_cmpd_4MesTer
_cod_database_code               7710536
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.499
_shelx_estimated_absorpt_t_min   0.352
_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
 P1-H1B = P1-H1A
 1.25 with sigma of 0.02
 P1-O1A
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(P1) = Uanis(O1) = Uanis(O1A)
4. Others
 Fixed Sof: O1A(0.5) O1(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C3(H3), C9(H9), C18(H18), C5(H5), C20(H20), C4(H4)
5.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C22(H22A,H22B,
 H22C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              92562
_shelx_hkl_checksum              48757
_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 6
_stoe_evaluation_lana_bos_l_odd_max 3
_stoe_evaluation_lana_completeness 98.8
_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 58.5
_stoe_evaluation_lana_max_2theta_desired 58.5
_stoe_evaluation_lana_mean_redundancy 2.6
_stoe_evaluation_lana_number_refls_after_or 20201
_stoe_evaluation_lana_number_refls_outliers 1311
_stoe_evaluation_lana_number_refls_total 21512
_stoe_evaluation_lana_number_refls_unique 7711
_stoe_evaluation_lana_number_refls_written 20201
_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           6.1   12.3   18.5   24.7   30.9   37.1   43.3   49.5   55.7
<Resolution>    5.73   3.17   2.17   1.65   1.33   1.11   0.96   0.85   0.76
N(total)         106    384    833   1444   2140   3025   3826   4858   4896
<Redundancy>     2.8    2.9    2.8    2.7    2.6    2.6    2.6    2.6    2.6
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0  100.0   95.1
<I/sigma>      449.5  294.5  173.3   98.3   55.2   27.7   11.9    4.7    2.0
R(int)         0.008  0.008  0.008  0.010  0.011  0.016  0.026  0.055  0.121
;
_stoe_measurement_identifier     ks1566
_stoe_measurement_max_exposure_per_frame '180.0 s'
_stoe_measurement_mean_exposure_per_frame '180.0 s'
_stoe_measurement_min_exposure_per_frame '180.0 s'
_stoe_measurement_total_exposure_time '13.9 h'
_stoe_measurement_total_frame_number 279
_stoe_measurement_total_run_number 2
_stoe_measurement_tube_power     '1.5 kW'