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_7133149
_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         'C47 H52 N2 O3 P, C32 H12 B F24'
_chemical_formula_sum            'C79 H64 B F24 N2 O3 P'
_chemical_formula_weight         1587.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-24
_audit_creation_method
;FinalCif V137 by Daniel Kratzert, Freiburg 2024, 
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                90
_cell_angle_beta                 97.228(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3660(8)
_cell_length_b                   20.9073(15)
_cell_length_c                   29.743(2)
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.465
_cell_measurement_theta_min      2.388
_cell_volume                     7628.6(9)
_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_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            173402
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.553
_diffrn_reflns_theta_min         1.925
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.8135
_exptl_absorpt_correction_T_min  0.7868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1078 before and 0.0441 after correction.
The Ratio of minimum to maximum transmission is 0.9672.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       block
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.626
_exptl_crystal_size_mid          0.574
_exptl_crystal_size_min          0.328
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         25477
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+3.3030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20853
_reflns_number_total             25477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02202e2.cif
_cod_data_source_block           mo_1866_cg_relabel
_cod_depositor_comments
'Adding full bibliography for 7133142--7133149.cif.'
_cod_original_cell_volume        7628.7(9)
_cod_database_code               7133149
_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
 C54-F1A \\sim C54-F3B
 with sigma of 0.04
 C54-F3A \\sim C54-F1B
 with sigma of 0.02
 F1A-F2A \\sim F3B-F2B
 with sigma of 0.02
 C54-F2A \\sim C54-F2B
 with sigma of 0.04
 F7A-C62 \\sim F7B-C62
 with sigma of 0.02
 F9A-C62 \\sim F8B-C62
 with sigma of 0.02
 F8A-C62 \\sim F9B-C62
 with sigma of 0.02
 F20A-C78 \\sim F20B-C78
 with sigma of 0.02
 F21A-C78 \\sim F21B-C78
 with sigma of 0.02
 F19A-C78 \\sim F19B-C78
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F21A, C78, F19A, F20A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
 F20B, C78, F21B, F19B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
4. Others
 1*[Sof(F1A)+Sof(F2A)+Sof(F3A)]+1*[Sof(F3B)+Sof(F2B)+Sof(F1B)]+1*[Sof(F28)+
 Sof(F29)+Sof(F30)]=1 with esd of 0.00001
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Sof(F3B)=Sof(F2B)=Sof(F1B)=FVAR(2)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=1-FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=FVAR(3)
 Sof(F19B)=Sof(F21B)=Sof(F20B)=1-FVAR(4)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=FVAR(4)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(5)
5.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C24(H24), C20(H20), C19(H19), C18(H18), C17(H17), C3(H3), C5(H5),
 C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
  C49(H49), C51(H51), C53(H53), C57(H57), C59(H59), C61(H61), C65(H65),
 C67(H67), C69(H69), C73(H73), C75(H75), C77(H77)
5.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C13(H13A,H13B,H13C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.954
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              39454
_shelx_hkl_checksum              34454