P(V)-bis(amidophenolate) ligand cooperation: stoichiometric CO-bond cleavage in aldehydes and ketones.
Karnbrock, Simon B. H.; Golz, Christopher; Alcarazo, Manuel; Chemical communications (Cambridge, England) 60 (2024) 6745–6748; doi:10.1039/d4cc02202e

data_7133142
_publ_section_title
;
 P(V)-bis(amidophenolate) ligand cooperation: stoichiometric
 C&#xe001;O-bond cleavage in aldehydes and ketones.
;
_journal_issue                   53
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6745
_journal_page_last               6748
_journal_paper_doi               10.1039/d4cc02202e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C1 H1 Cl3, C37 H50 N2 O3 P, C32 H12 B F24'
_chemical_formula_sum            'C70 H63 B Cl3 F24 N2 O3 P'
_chemical_formula_weight         1584.35
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-14
_audit_creation_method
;FinalCif V113 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-05-06 deposited with the CCDC.	2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                81.400(2)
_cell_angle_beta                 78.136(2)
_cell_angle_gamma                78.970(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6492(9)
_cell_length_b                   13.6605(10)
_cell_length_c                   21.8343(14)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.755
_cell_measurement_theta_min      2.303
_cell_volume                     3600.1(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker BIS V6.2.14/2020-04-30'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            91367
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.739
_diffrn_reflns_theta_min         1.919
_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    0.259
_exptl_absorpt_correction_T_max  0.6847
_exptl_absorpt_correction_T_min  0.6201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0976 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.9057.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         18627
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0510P)^2^+3.3276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15593
_reflns_number_total             18627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02202e2.cif
_cod_data_source_block           mo_1848_sk_0m
_cod_depositor_comments
'Adding full bibliography for 7133142--7133149.cif.'
_cod_database_code               7133142
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1A-C70A \\sim Cl1B-C70B
 with sigma of 0.02
 Cl2A-Cl3A \\sim Cl2B-Cl3B
 with sigma of 0.04
 Cl3A-C70A \\sim Cl3B-C70B
 with sigma of 0.02
 Cl2A-C70A \\sim Cl2B-C70B
 with sigma of 0.02
 Cl1A-Cl2A \\sim Cl1B-Cl2B
 with sigma of 0.04
 Cl1A-Cl3A \\sim Cl1B-Cl3B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F15A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
F14A \\sim F13B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F13A \\sim F15B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F15A \\sim F14B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C70A \\sim C70B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
Cl1A \\sim Cl1B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
Cl2A \\sim Cl2B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
4. Rigid body (RIGU) restrains
 C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1A, Cl2A, Cl3A, C70A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1B, Cl2B, Cl3B, C70B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F15A, F14A, F13A, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F13B, F14B, F15B, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F15A)=Sof(F14A)=Sof(F13A)=1-FVAR(1)
 Sof(F13B)=Sof(F14B)=Sof(F15B)=FVAR(1)
 Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=Sof(C70B)=Sof(H70B)=1-FVAR(2)
 Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=Sof(C70A)=Sof(H70A)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C70A(H70A), C70B(H70B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C19(H19), C20(H20), C21(H21), C22(H22), C27(H27), C29(H29),
 C39(H39), C41(H41), C43(H43), C47(H47), C49(H49), C51(H51), C55(H55), C57(H57),
  C59(H59), C63(H63), C65(H65), C67(H67)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.967
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              46655
_shelx_hkl_checksum              11123