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_7714928
_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         'C28 H22 N2 O5 P W, C F3 O3 S, 0.25(C5 H12)'
_chemical_formula_sum            'C30.25 H25 F3 N2 O8 P S W'
_chemical_formula_weight         848.40
_chemical_name_systematic        DB-571-2
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-11-29
_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                 125.097(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   54.221(3)
_cell_length_b                   8.9542(5)
_cell_length_c                   32.5364(19)
_cell_measurement_reflns_used    9218
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.279
_cell_measurement_theta_min      2.538
_cell_volume                     12924.5(13)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.999
_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  0.0551
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       74
_diffrn_reflns_limit_h_min       -74
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            145150
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.250
_diffrn_reflns_theta_min         1.836
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.758
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1062 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.7830.
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    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             6664
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.908
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         17600
_refine_ls_number_restraints     942
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+184.8187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15648
_reflns_number_total             17600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03869f2.cif
_cod_data_source_block           11a
_cod_depositor_comments
'Adding full bibliography for 7714921--7714928.cif.'
_cod_database_code               7714928
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.466
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29T-F1T = C29T-F3T = C29T-F2T
 1.33 with sigma of 0.02
 C29T-ST
 1.82 with sigma of 0.02
 ST-O6T = ST-O7T = ST-O8T
 1.44 with sigma of 0.02
 C29S-F3S = C29S-F2S = C29S-F1S
 1.33 with sigma of 0.02
 C29S-SS
 1.82 with sigma of 0.02
 SS-O7S = SS-O8S = SS-O6S
 1.44 with sigma of 0.02
 H-P
 1.5 with sigma of 0.02
 H'-P'
 1.5 with sigma of 0.02
 C34-C33 = C33-C32 = C32-C31 = C31-C30
 1.52 with sigma of 0.001
 C34-C32 = C33-C31 = C32-C30
 2.54 with sigma of 0.001
 C29T-O7T
 2.56 with sigma of 0.04
 C29T-O6T
 2.58 with sigma of 0.04
 C29T-O8T
 2.57 with sigma of 0.04
 C29S-O7S
 2.58 with sigma of 0.04
 C29S-O8S
 2.56 with sigma of 0.04
 C29S-O6S
 2.57 with sigma of 0.04
 F1T-F2T \\sim F2T-F3T \\sim F3T-F1T
 with sigma of 0.001
 O6S-O7S \\sim O7S-O8S \\sim O8S-O6S
 with sigma of 0.001
3. Rigid bond restraints
 P', N1'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(N1') \\sim Ueq, Uanis(C3') \\sim Ueq, Uanis(C2') \\sim Ueq, Uanis(N2')
\\sim Ueq, Uanis(C1') \\sim Ueq, Uanis(C4') \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C23') \\sim Ueq, Uanis(C21') \\sim Ueq, Uanis(C22') \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(F2T) \\sim Ueq, Uanis(C29T) \\sim Ueq, Uanis(F3T) \\sim Ueq, Uanis(F1T)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: SS(0.5) F1S(0.5) F2S(0.5) F3S(0.5) O6S(0.5) O7S(0.5) O8S(0.5)
 C29S(0.5) ST(0.5) F1T(0.5) F2T(0.5) F3T(0.5) O6T(0.5) O7T(0.5) O8T(0.5)
 C29T(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 C32(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5)
 H34B(0.5) H34C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C1'(H1'), C2'(H2'), C3'(H3'), C7'(H7'), C8'(H8'), C9'(H9'),
 C10'(H10'), C11'(H11'), C13'(H13'), C14'(H14'), C15'(H15'), C16'(H16'),
 C17'(H17'), C19'(H19'), C20'(H20'), C21'(H21'), C22'(H22'), C23'(H23')
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C4'(H4'A,H4'B,H4'C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              67072
_shelx_hkl_checksum              43413
_olex2_submission_special_instructions 'No special instructions were received'