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_1560095
_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         'C36 H53 B N6 O3 P2 Pd W'
_chemical_formula_sum            'C36 H53 B N6 O3 P2 Pd W'
_chemical_formula_weight         980.84
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8853(7)
_cell_length_b                   15.2569(7)
_cell_length_c                   15.7122(8)
_cell_measurement_reflns_used    3932
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.20
_cell_volume                     4046.0(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30841
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         1.799
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.406
_exptl_absorpt_correction_T_max  0.3812
_exptl_absorpt_correction_T_min  0.3065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0753 before and 0.0558 after correction.
The Ratio of minimum to maximum transmission is 0.8164.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       prism
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.446
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0277P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7383
_reflns_number_total             9756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06114j2.cif
_cod_data_source_block           kg02
_cod_depositor_comments
'Adding full bibliography for 1560095--1560096.cif.'
_cod_database_code               1560095
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.483
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 B1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36)
2.d 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)
;
_shelx_res_checksum              57407
_olex2_submission_special_instructions 'No special instructions were received'