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_7710532
_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         'C35 H50 Cl7 Ga P2'
_chemical_formula_sum            'C35 H50 Cl7 Ga P2'
_chemical_formula_weight         850.56
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,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             2022-06-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-06-21 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.350(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0543(14)
_cell_length_b                   25.215(2)
_cell_length_c                   16.013(3)
_cell_measurement_reflns_used    5954
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      1.98
_cell_volume                     4436.0(11)
_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)'
_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
;
 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  0.0277
_diffrn_reflns_av_unetI/netI     0.0173
_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       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57514
_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         26.498
_diffrn_reflns_theta_min         1.513
_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    1.136
_exptl_absorpt_correction_T_max  0.6088
_exptl_absorpt_correction_T_min  0.4610
_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    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_crystal_size_rad          0.089
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         9185
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1043
_reflns_d_resolution_high        0.757
_reflns_d_resolution_low         13.459
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              33
_reflns_limit_k_min              -33
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                7636
_reflns_number_total             9185
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d2dt01575g2.cif
_cod_data_source_block           ks1575
_cod_original_cell_volume        4436.1(10)
_cod_database_code               7710532
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.720
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl7-C36A = Cl6-C36A = Cl6-C36 = Cl7-C36
 1.8 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C36) = Uanis(C36A)
4. Others
 Sof(H35C)=Sof(H35D)=Sof(Cl9A)=1-FVAR(1)
 Sof(H35A)=Sof(H35B)=Sof(Cl9)=FVAR(1)
 Sof(C36)=Sof(H36C)=Sof(H36D)=1-FVAR(2)
 Sof(C36A)=Sof(H36A)=Sof(H36B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C25(H25), C13(H13), C16(H16), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C35(H35C,H35D), C35(H35A,H35B), C36A(H36A,H36B), C36(H36C,H36D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4), C22(H22), C21(H21), C23(H23), C10(H10), C9(H9),
 C11(H11)
5.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,
 H18B,H18C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C17(H17A,H17B,H17C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57508
_shelx_hkl_checksum              13361
_shelx_fab_checksum              42108
_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 98.3
_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 56.2
_stoe_evaluation_lana_max_2theta_desired 56.2
_stoe_evaluation_lana_mean_redundancy 6.3
_stoe_evaluation_lana_number_refls_after_or 66969
_stoe_evaluation_lana_number_refls_outliers 9416
_stoe_evaluation_lana_number_refls_total 76385
_stoe_evaluation_lana_number_refls_unique 10649
_stoe_evaluation_lana_number_refls_written 66969
_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           5.6   11.6   17.6   23.6   29.6   35.6   41.6   47.6   53.6
<Resolution>    6.13   3.36   2.28   1.72   1.38   1.16   1.00   0.88   0.79
N(total)         306   1272   2869   5025   7719  10615  13941  17143  17495
<Redundancy>     5.3    5.7    5.6    5.7    5.9    6.1    6.3    6.6    6.6
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0  100.0   93.5
<I/sigma>      367.8  280.9  121.1   82.0   38.8   22.2   12.4    6.2    3.0
R(int)         0.014  0.017  0.018  0.017  0.021  0.029  0.041  0.067  0.119
;
_stoe_measurement_identifier     ks1575
_stoe_measurement_max_exposure_per_frame '120.0 s'
_stoe_measurement_mean_exposure_per_frame '120.0 s'
_stoe_measurement_min_exposure_per_frame '120.0 s'
_stoe_measurement_total_exposure_time '12.0 h'
_stoe_measurement_total_frame_number 360
_stoe_measurement_total_run_number 2
_stoe_measurement_tube_power     '1.5 kW'