Low-coordinate bis-phosphine and monophosphine Ni(0) complexes: synthesis and reactivity in C-S cross-coupling.
Martín, M Trinidad; Carrasco, Carlos J.; Santamaría, Nazaret; Maya, Celia; Prieto, Auxiliadora; Galindo, Agustín; Nicasio, M. Carmen; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2645–2653; doi:10.1039/d4dt03375b

data_7718239
_publ_section_title
;
 Low-coordinate bis-phosphine and monophosphine Ni(0) complexes: synthesis
 and reactivity in C-S cross-coupling.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2645
_journal_page_last               2653
_journal_paper_doi               10.1039/d4dt03375b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C28 H37 Ni O P Si2'
_chemical_formula_sum            'C28 H37 Ni O P Si2'
_chemical_formula_weight         535.43
_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_date             2024-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-25 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.859(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.534(2)
_cell_length_b                   9.7686(7)
_cell_length_c                   21.7530(18)
_cell_measurement_reflns_used    3060
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.69
_cell_measurement_theta_min      2.45
_cell_volume                     5647.5(8)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13264
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         22.101
_diffrn_reflns_theta_min         1.558
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1017 before and 0.0310 after correction.
The Ratio of minimum to maximum transmission is 0.7365.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       prism
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0463P)^2^+8.9935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3930
_reflns_number_total             6349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03375b3.cif
_cod_data_source_block           5
_cod_database_code               7718239
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.901
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C22(H22), C27(H27)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
1.c X=CH2 refined with riding coordinates:
 C21(H21A,H21B), C28(H28A,H28B)
1.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              81333
_olex2_submission_special_instructions 'No special instructions were received'