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_7710535
_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         'C36 H60 O P2'
_chemical_formula_sum            'C36 H60 O P2'
_chemical_formula_weight         570.78
_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             2022-03-05
_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                 99.501(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2606(7)
_cell_length_b                   10.4141(8)
_cell_length_c                   30.070(2)
_cell_measurement_reflns_used    5098
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      60.071
_cell_measurement_theta_min      2.980
_cell_volume                     3477.9(4)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX II Duo'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.1200
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5098
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        60.071
_diffrn_reflns_theta_max         60.071
_diffrn_reflns_theta_min         2.980
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.785
_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    1.090
_exptl_crystal_description       needle
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0848
_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^)+(0.1108P)^2^+1.2967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3596
_reflns_number_total             5098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01575g2.cif
_cod_data_source_block           fdpx10_cmpd_2MesStar
_cod_database_code               7710535
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.920(2)
 0.080(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Everything fixed:
 H1, H2
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C23(H23), C21(H21)
3.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C14(H14A,H14B,
 H14C), C10(H10A,H10B,H10C), C28(H28A,H28B,H28C), C17(H17A,H17B,H17C), C8(H8A,
 H8B,H8C), C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C27(H27A,
 H27B,H27C), C31(H31A,H31B,H31C), C36(H36A,H36B,H36C), C30(H30A,H30B,H30C),
 C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              63571
_shelx_hkl_checksum              77065
_olex2_submission_special_instructions 'No special instructions were received'