Aryl group transfer and C–P bond formation in the reaction of organonickel complexes with sodium 3,4,5-triphenyl-1,2-diphospholide
Sakhapov, I. F.; Zagidullin, A. A.; Gafurov, Z. N.; Khismatova, D. K.; Zaripov, R. B.; Kagilev, A. A.; Kantyukov, A. O.; Zueva, E. M.; Petrova, M. M.; Litvinov, I. A.; Miluykov, V. A.; Shmelev, A. G.; Sinyashin, O. G.; Yakhvarov, D. G.; New Journal of Chemistry 48 (2024) 1559–1566; doi:10.1039/D3NJ04924H

data_7062917
_publ_section_title
;
 Aryl group transfer and C--P bond formation in the reaction of
 organonickel complexes with sodium 3,4,5-triphenyl-1,2-diphospholide
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1559
_journal_page_last               1566
_journal_paper_doi               10.1039/D3NJ04924H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         ' C30 H26 P2, 0.5(C10 H8 N2)'
_chemical_formula_sum            'C35 H30 N P2'
_chemical_formula_weight         526.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-04-11 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.6830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.2770(8)
_cell_length_b                   15.3360(6)
_cell_length_c                   17.4979(11)
_cell_measurement_reflns_used    9557
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.40
_cell_volume                     5659.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100232
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.141
_diffrn_reflns_theta_min         1.931
_diffrn_source                   'I\mS DIAMOND'
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6014
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       formless
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         7592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0564P)^2^+3.7324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6325
_reflns_number_total             7592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04924h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7062917.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7062917
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              15543
_shelx_hkl_checksum              58629