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_7133145
_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         'C52 H70 N4 O3 P, C32 H12 B F24, 1[CH3CN]'
_chemical_formula_sum            'C86 H85 B F24 N5 O3 P'
_chemical_formula_weight         1734.36
_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             2023-06-16
_audit_creation_method
;FinalCif V122 by Daniel Kratzert, Freiburg 2023, 
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                70.624(3)
_cell_angle_beta                 73.911(4)
_cell_angle_gamma                75.970(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1449(17)
_cell_length_b                   18.623(3)
_cell_length_c                   20.405(3)
_cell_measurement_reflns_used    9739
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.831
_cell_measurement_theta_min      2.170
_cell_volume                     4125.1(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
'Bruker BIS V6.2.15/2021-03-16 && APEX4 2022.1-1'
_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_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 0.991
_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  0.0523
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89259
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.886
_diffrn_reflns_theta_min         1.955
_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    0.140
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7890
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1547 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.7890.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_recrystallization_method
'from a mixture of chloroform, pentane and acetonitrile.'
_exptl_crystal_size_max          0.578
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         21505
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0711P)^2^+2.8552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16187
_reflns_number_total             21505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02202e2.cif
_cod_data_source_block           mo_2007_cg_0m
_cod_depositor_comments
'Adding full bibliography for 7133142--7133149.cif.'
_cod_original_cell_volume        4125.2(10)
_cod_database_code               7133145
_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
 F13A-C75 \\sim F13B-C75
 with sigma of 0.02
 F3A-C59A \\sim F3B-C59B
 with sigma of 0.02
 F15A-C75 \\sim F15B-C75
 with sigma of 0.02
 F1A-F3A \\sim F1B-F3B
 with sigma of 0.04
 F2A-F3A \\sim F2B-F3B
 with sigma of 0.04
 F3A-C57 \\sim F3B-C57
 with sigma of 0.04
 F14A-C75 \\sim F14B-C75
 with sigma of 0.02
 F1A-C59A \\sim F1B-C59B
 with sigma of 0.02
 F2A-C59A \\sim F2B-C59B
 with sigma of 0.02
 C57-C59A \\sim C57-C59B
 with sigma of 0.02
 F1A-F2A \\sim F1B-F2B
 with sigma of 0.04
 F1A-C57 \\sim F1B-C57
 with sigma of 0.04
 F2A-C57 \\sim F2B-C57
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 F13A, F14A, F15A, C75
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.001
 F13B, F14B, F15B, C75
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.001
 F1B, F2B, F3B, C57, C59B
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.001
 F1A, F2A, F3A, C57, C59A
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.001
 F22, F23, F24, C84
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C84
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(F13B)=Sof(F14B)=Sof(F15B)=1-FVAR(1)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(C59B)=1-FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C59A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C35(H35), C38(H38), C40(H40), C43(H43)
5.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,
 H44B), C45(H45A,H45B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C31(H31), C32(H32), C33(H33), C34(H34),
 C46(H46), C47(H47), C49(H49), C50(H50), C54(H54), C56(H56), C58(H58), C62(H62),
  C64(H64), C66(H66), C70(H70), C72(H72), C74(H74), C78(H78), C80(H80), C82(H82)
5.d 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), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.993
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              38439
_shelx_hkl_checksum              94292
_shelx_fab_checksum              75249