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_7710541
_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         'C33 H47 P2, Cl4 Ga'
_chemical_formula_sum            'C33 H47 Cl4 Ga P2'
_chemical_formula_weight         717.16
_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                92.053(2)
_cell_angle_beta                 104.767(2)
_cell_angle_gamma                104.411(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7565(3)
_cell_length_b                   11.7069(4)
_cell_length_c                   17.4299(6)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      66.57
_cell_measurement_theta_min      2.64
_cell_volume                     1853.99(11)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23411
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.613
_diffrn_reflns_theta_max         66.613
_diffrn_reflns_theta_min         2.636
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.629
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'APEX2, SADABS was used for absorption correction.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6527
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0546P)^2^+1.2837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5663
_reflns_number_total             6527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01575g2.cif
_cod_data_source_block           ax2299abs_cmpd_12DipTer
_cod_database_code               7710541
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.630
_shelx_estimated_absorpt_t_min   0.302
_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
 Ga1-Cl2A
 2.18 with sigma of 0.001
 Ga1-Cl1A = Ga1-Cl4A
 2.18 with sigma of 0.007
 Ga1-Cl4A = Ga1-Cl1A
 2.18 with sigma of 0.004
 Cl2-Ga1
 2.18 with sigma of 0.005
 Ga1-Cl2
 2.18 with sigma of 0.001
 Cl3A-Cl1A
 3.5 with sigma of 0.01
 Cl4A-Cl3A
 3.5 with sigma of 0.01
 Cl4-Cl2
 3.5 with sigma of 0.01
 Cl4-Cl3
 3.5 with sigma of 0.01
 Cl2-Cl3
 3.5 with sigma of 0.01
 Cl4A-Cl1A
 3.5 with sigma of 0.01
 Cl3-Cl1
 3.5 with sigma of 0.01
 Cl4A-Cl2A
 3.5 with sigma of 0.01
 Cl1-Cl2
 3.5 with sigma of 0.01
 Cl4-Cl1
 3.5 with sigma of 0.01
 Cl2A-Cl3A
 3.5 with sigma of 0.01
 P1-H1A \\sim P1-H1B
 with sigma of 0.02
 Ga1-Cl4 \\sim Ga1-Cl4A
 with sigma of 0.02
 Ga1-Cl2 \\sim Ga1-Cl2A
 with sigma of 0.01
 Ga1-Cl3 \\sim Ga1-Cl3A
 with sigma of 0.01
 Ga1-Cl1 \\sim Ga1-Cl1A
 with sigma of 0.01
 Ga1-Cl4A \\sim Ga1-Cl4
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C31) = Uanis(C31A)
4. Others
 Sof(P2A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C31A)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(H1B)=1-FVAR(1)
 Sof(P2)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=
 Sof(H33C)=Sof(C31)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(H1A)=FVAR(1)
 Sof(Cl2)=Sof(Cl1)=Sof(Cl3)=Sof(Cl4)=1-FVAR(2)
 Sof(Cl2A)=Sof(Cl1A)=Sof(Cl4A)=Sof(Cl3A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C28(H28), C16(H16), C25(H25), C13(H13)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C21(H21), C23(H23), C9(H9), C4(H4), C22(H22), C10(H10),
 C11(H11)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C26(H26A,H26B,
 H26C), C18(H18A,H18B,H18C), C32(H32A,H32B,H32C), C17(H17A,H17B,H17C), C33(H33A,
 H33B,H33C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C32A(H32D,H32E,H32F),
 C31A(H31A,H31B,H31C), C31(H31D,H31E,H31F), C33A(H33D,H33E,H33F)
;
_shelx_res_checksum              35313
_shelx_hkl_checksum              9110
_olex2_submission_special_instructions 'No special instructions were received'