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_7718241
_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         'C32 H45 Ni O P Si2, 1[C4H10O]'
_chemical_formula_sum            'C36 H55 Ni O2 P Si2'
_chemical_formula_weight         665.66
_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
_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                 112.336(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.527(3)
_cell_length_b                   23.642(6)
_cell_length_c                   14.134(3)
_cell_measurement_reflns_used    9383
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.11
_cell_measurement_theta_min      2.38
_cell_volume                     3871.9(16)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.1256
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            208312
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.499
_diffrn_reflns_theta_min         1.405
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.7285
_exptl_absorpt_correction_T_min  0.6682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1160 before and 0.0859 after correction.
The Ratio of minimum to maximum transmission is 0.9172.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         7899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0461P)^2^+1.7341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6730
_reflns_number_total             7899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03375b3.cif
_cod_data_source_block           6
_cod_original_cell_volume        3871.7(16)
_cod_database_code               7718241
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.934
_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. Others
 Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(Si1A)=Sof(O1A)=Sof(Si2A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=
 Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(Si1)=Sof(Si2)=Sof(O1)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C26(H26), C31(H31)
3.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C32(H32A,H32B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18),
 C19(H19)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C30B(H30D,H30E,H30F),
 C29B(H29D,H29E,H29F), C28A(H28D,H28E,H28F), C27A(H27D,H27E,H27F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44108
_shelx_fab_checksum              61097
_olex2_submission_special_instructions 'No special instructions were received'