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_7710531
_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         'Cl4 Ga, C27 H35 P2'
_chemical_formula_sum            'C27 H35 Cl4 Ga P2'
_chemical_formula_weight         633.01
_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   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
;
2022-04-14 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.478(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2634(4)
_cell_length_b                   13.3291(7)
_cell_length_c                   28.2426(13)
_cell_measurement_reflns_used    29266
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      1.42
_cell_volume                     3109.7(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 360 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  0.0278
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            42012
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.442
_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    1.346
_exptl_absorpt_correction_T_max  0.6082
_exptl_absorpt_correction_T_min  0.5652
_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    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_crystal_size_rad          0.078
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+9.6755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1378
_reflns_d_resolution_high        0.758
_reflns_d_resolution_low         14.117
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              37
_reflns_limit_l_min              -37
_reflns_number_gt                5243
_reflns_number_total             6455
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d2dt01575g2.cif
_cod_data_source_block           ks1570_cmpd_12MesTer
_cod_database_code               7710531
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.747
_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.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C18(H18), C9(H9), C20(H20), C5(H5), C3(H3), C4(H4)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C15(H15A,H15B,H15C), C26(H26A,H26B,
 H26C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C14(H14A,H14B,H14C), C22(H22A,
 H22B,H22C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              2032
_shelx_hkl_checksum              19921
_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 98.6
_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 6.4
_stoe_evaluation_lana_number_refls_after_or 49318
_stoe_evaluation_lana_number_refls_outliers 4300
_stoe_evaluation_lana_number_refls_total 53618
_stoe_evaluation_lana_number_refls_unique 7763
_stoe_evaluation_lana_number_refls_written 49318
_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           5.5   11.5   17.5   23.5   29.5   35.5   41.5   47.5   53.5
<Resolution>    6.15   3.40   2.29   1.73   1.38   1.16   1.00   0.88   0.79
N(total)         241    896   2014   3520   5451   7511   9780  11964  12241
<Redundancy>     5.4    6.0    5.8    6.0    6.1    6.3    6.4    6.6    6.4
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.1   99.9  100.0   94.5
<I/sigma>      306.6  186.9   91.6   70.6   31.6   17.1    9.6    4.4    1.8
R(int)         0.010  0.013  0.014  0.015  0.020  0.029  0.047  0.091  0.184
;
_stoe_measurement_identifier     ks1570
_stoe_measurement_max_exposure_per_frame '600.0 s'
_stoe_measurement_mean_exposure_per_frame '600.0 s'
_stoe_measurement_min_exposure_per_frame '600.0 s'
_stoe_measurement_total_exposure_time '60.0 h'
_stoe_measurement_total_frame_number 360
_stoe_measurement_total_run_number 2
_stoe_measurement_tube_power     '1.5 kW'