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_7714927
_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         'C32 H12 B F24, C28 H22 N2 O5 P W, C H2 Cl2'
_chemical_formula_sum            'C61 H36 B Cl2 F24 N2 O5 P W'
_chemical_formula_weight         1629.45
_chemical_name_systematic        DB-604
_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             2022-12-13
_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                98.0490(10)
_cell_angle_beta                 104.5540(10)
_cell_angle_gamma                94.751(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3237(5)
_cell_length_b                   14.0365(6)
_cell_length_c                   20.5226(7)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.484
_cell_measurement_theta_min      2.523
_cell_volume                     3102.4(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0233
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89491
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.942
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.097
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0937 before and 0.0387 after correction. The Ratio of minimum to maximum transmission is 0.8483. 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       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         14911
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0188
_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^)+(0.0183P)^2^+2.9212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14610
_reflns_number_total             14911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03869f2.cif
_cod_data_source_block           11b
_cod_depositor_comments
'Adding full bibliography for 7714921--7714928.cif.'
_cod_database_code               7714927
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.655
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
F15 \\sim F14S \\sim F14 \\sim F13S \\sim F13 \\sim F15S: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(F13S) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F14S) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F15S) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F24) \\sim Ueq,
Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl2S)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F24S) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F22S) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(F23S) \\sim Ueq, Uanis(F23) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(F15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(F13S)=Sof(F14S)=Sof(F15S)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
 Sof(Cl2S)=Sof(H61C)=Sof(H61D)=1-FVAR(2)
 Sof(Cl2)=Sof(H61A)=Sof(H61B)=FVAR(2)
 Sof(F22S)=Sof(F23S)=Sof(F24S)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C61(H61C,H61D)
4.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), C30(H30), C32(H32), C34(H34), C38(H38), C40(H40), C42(H42),
 C46(H46), C48(H48), C50(H50), C54(H54), C56(H56), C58(H58)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              25709
_shelx_hkl_checksum              61059
_olex2_submission_special_instructions 'No special instructions were received'