Bifunctional activation of amine-boranes by the W/Pd bimetallic analogs of “frustrated Lewis pairs”
Osipova, Elena S.; Gulyaeva, Ekaterina S.; Gutsul, Evgenii I.; Kirkina, Vladislava A.; Pavlov, Alexander A.; Nelyubina, Yulia V.; Rossin, Andrea; Peruzzini, Maurizio; Epstein, Lina M.; Belkova, Natalia V.; Filippov, Oleg A.; Shubina, Elena S.; Chemical Science 12 (2021) 3682–3692; doi:10.1039/D0SC06114J

data_1560096
_publ_section_title
;
 Bifunctional activation of amine-boranes by the W/Pd bimetallic analogs
 of &#x201C;frustrated Lewis pairs&#x201D;
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3682
_journal_page_last               3692
_journal_paper_doi               10.1039/D0SC06114J
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C32 H48 O3 P2 Pd W'
_chemical_formula_sum            'C32 H48 O3 P2 Pd W'
_chemical_formula_weight         832.89
_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             2020-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.3880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2012(2)
_cell_length_b                   37.3720(8)
_cell_length_c                   10.9355(2)
_cell_measurement_reflns_used    4255
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.37
_cell_measurement_theta_min      2.36
_cell_volume                     3260.59(12)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            45938
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         2.364
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.032
_exptl_absorpt_correction_T_max  0.4672
_exptl_absorpt_correction_T_min  0.2895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1302 before and 0.0840 after correction.
The Ratio of minimum to maximum transmission is 0.6196.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.702
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.00031(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5834
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0406P)^2^+10.7029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4578
_reflns_number_total             5834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06114j2.cif
_cod_data_source_block           kg01
_cod_depositor_comments
'Adding full bibliography for 1560095--1560096.cif.'
_cod_database_code               1560096
_shelxl_version_number           2014/6
_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. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'