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_7714921
_publ_section_title
;
 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         '2(C24 H17 O6 P W), C4 H8 O'
_chemical_formula_sum            'C52 H42 O13 P2 W2'
_chemical_formula_weight         1304.49
_chemical_name_systematic        DB-403
_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             2023-10-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                97.985(3)
_cell_angle_beta                 91.166(4)
_cell_angle_gamma                109.171(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3995(9)
_cell_length_b                   11.6790(10)
_cell_length_c                   12.0501(11)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.81
_cell_measurement_theta_min      2.33
_cell_volume                     1234.3(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.969
_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_unetI/netI     0.0860
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.868
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.786
_exptl_absorpt_correction_T_max  0.745472
_exptl_absorpt_correction_T_min  0.588614
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1118 before and 0.0676 after correction.
 The Ratio of minimum to maximum transmission is 0.79.

Final HKLF 4 output contains 96125 reflections, Rint = 0.1977
 (30273 with I > 3sig(I), Rint = 0.1238)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.081
_refine_diff_density_min         -2.819
_refine_diff_density_rms         0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4891
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0125P)^2^+18.8775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4361
_reflns_number_total             4891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03869f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7714921--7714928.cif.'
_cod_database_code               7714921
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.448
_shelx_estimated_absorpt_t_min   0.251
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.592(6)
 0.093(3) 0.181(3) 0.109(3) 0.025(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 O7-C28 = O7-C25
 1.44 with sigma of 0.02
 C28-C27 = C26-C25
 1.53 with sigma of 0.02
 C27-C26
 1.54 with sigma of 0.02
 O7-C27 = O7-C26 = C28-C26 = C27-C25
 2.38 with sigma of 0.04
 C27-C25 \\sim C28-C26
 with sigma of 0.04
 O7-C27 \\sim O7-C26
 with sigma of 0.04
 C28-C27 \\sim C27-C26 \\sim C26-C25
 with sigma of 0.02
 O7-C28 \\sim O7-C25
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O7 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C27 \\sim C26 \\sim C28 \\sim O7: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Uanis(C25) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C27) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 O7, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O7(0.5) C25(0.5) H25A(0.5) H25B(0.5) C26(0.5) H26A(0.5) H26B(0.5)
 C27(0.5) H27A(0.5) H27B(0.5) C28(0.5) H28A(0.5) H28B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
7.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              26401
_shelx_hkl_checksum              67086
_olex2_submission_special_instructions 'No special instructions were received'