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_7718240
_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         'C60 H46 Ni O4 P2'
_chemical_formula_sum            'C60 H46 Ni O4 P2'
_chemical_formula_weight         951.62
_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             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                 93.9410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9594(3)
_cell_length_b                   29.1507(7)
_cell_length_c                   13.3094(3)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.37
_cell_volume                     4629.02(19)
_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      193.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            75363
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         2.075
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0618 before and 0.0515 after correction.
The Ratio of minimum to maximum transmission is 0.9345.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       prism
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         10633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0327P)^2^+3.5115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9058
_reflns_number_total             10633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03375b3.cif
_cod_data_source_block           4
_cod_database_code               7718240
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C30(H30), C29(H29), C28(H28),
 C27(H27), C26(H26), C17(H17), C16(H16), C15(H15), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C39(H39), C40(H40), C41(H41), C50(H50),
  C51(H51), C52(H52), C53(H53), C54(H54), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
;
_shelx_res_checksum              55185
_olex2_submission_special_instructions 'No special instructions were received'