Access to ligand-stabilized PH-containing phosphenium complexes.
Biskup, David; Schnakenburg, Gregor; Espinosa Ferao, Arturo; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2517–2525; doi:10.1039/d3dt03869f

data_7714925
_publ_section_title
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 Access to ligand-stabilized PH-containing phosphenium complexes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2517
_journal_page_last               2525
_journal_paper_doi               10.1039/d3dt03869f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H22 N2 O5 P W'
_chemical_formula_sum            'C28 H22 N2 O5 P W'
_chemical_formula_weight         681.29
_chemical_name_systematic        DB-568
_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             2022-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.490(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9563(5)
_cell_length_b                   34.958(2)
_cell_length_c                   16.3809(13)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.433
_cell_measurement_theta_min      2.575
_cell_volume                     5652.8(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            137230
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.144
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.091
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0931 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.8700. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.801
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.265
_refine_diff_density_min         -1.883
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         13629
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0824
_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^)+(0.1194P)^2^+96.5095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2406
_refine_ls_wR_factor_ref         0.2447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12411
_reflns_number_total             13629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03869f2.cif
_cod_data_source_block           11c
_cod_depositor_comments
'Adding full bibliography for 7714921--7714928.cif.'
_cod_database_code               7714925
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.787
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P-H
 1.43 with sigma of 0.001
 W-H
 3 with sigma of 0.01
 H-N1
 3.3 with sigma of 0.1
 C5-H
 2.9 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C12 \\sim C12S \\sim C13 \\sim C13S \\sim C14 \\sim C14S \\sim C15 \\sim C15S
\\sim C16 \\sim C16S \\sim C17 \\sim C17S: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C28)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq, Uanis(C14S) \\sim Ueq, Uanis(C15S) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16S) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(C16S)=Sof(H16S)=Sof(C15S)=Sof(H15S)=Sof(C14S)=Sof(H14S)=Sof(C13S)=
 Sof(H13S)=Sof(C12S)=Sof(C17S)=Sof(H17S)=1-FVAR(1)
 Sof(C12)=Sof(C17)=Sof(H17)=Sof(C16)=Sof(H16)=Sof(C15)=Sof(H15)=Sof(C14)=
 Sof(H14)=Sof(C13)=Sof(H13)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C17(H17),
 C16(H16), C15(H15), C14(H14), C13(H13), C16S(H16S), C15S(H15S), C14S(H14S),
 C13S(H13S), C17S(H17S), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
5.b Fitted hexagon refined as free rotating group:
 C12(C17,C16,C15,C14,C13), C16S(C15S,C14S,C13S,C12S,C17S)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              56434
_shelx_hkl_checksum              12431
_shelx_fab_checksum              91459
_olex2_submission_special_instructions 'No special instructions were received'