Synthesis and catalytic performance of nickel phosphinite pincer complexes in deoxygenative hydroboration of amides
Adilkhanova, Aziza; Frolova, Valeriya F.; Yessengazin, Azamat; Öztopçu, Özgür; Gudun, Kristina A.; Segizbayev, Medet; Matsokin, Nikita A.; Dmitrienko, Anton; Pilkington, Melanie; Khalimon, Andrey Y.; Dalton Transactions 52 (2023) 2872–2886; doi:10.1039/D2DT03801C

data_7712451
_publ_section_title
;
 Synthesis and catalytic performance of nickel phosphinite pincer
 complexes in deoxygenative hydroboration of amides
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              2872
_journal_page_last               2886
_journal_paper_doi               10.1039/D2DT03801C
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C15 H25 N2 Ni O4 P'
_chemical_formula_sum            'C15 H25 N2 Ni O4 P'
_chemical_formula_weight         387.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2023-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.156(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2003(9)
_cell_length_b                   9.4423(8)
_cell_length_c                   16.3874(13)
_cell_measurement_reflns_used    458
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     1700.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector''
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_unetI/netI     0.0995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17214
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_min         2.439
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.442
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0267P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3413
_reflns_number_total             4953
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d2dt03801c2.cif
_cod_data_source_block           7
_cod_database_code               7712451
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.736
_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.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C15(H15A,H15B,
 H15C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              66155
_olex2_submission_special_instructions 'No special instructions were received'