Reactivity of low-valent nickel carbonyl species supported by acridane based PNP ligands towards iodoalkanes.
Park, Sanha; Seo, Mi Sook; Kim, Mingi; Lee, Kang Mun; Graham, Peter M.; Lee, Yunho; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10120–10125; doi:10.1039/d4dt01022a

data_7716197
_publ_section_title
;
 Reactivity of low-valent nickel carbonyl species supported by acridane
 based PNP ligands towards iodoalkanes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10120
_journal_page_last               10125
_journal_paper_doi               10.1039/d4dt01022a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C39 H48 N Ni P2'
_chemical_formula_sum            'C39 H48 N Ni P2'
_chemical_formula_weight         651.43
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-12 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                97.778(2)
_cell_angle_beta                 103.185(2)
_cell_angle_gamma                90.545(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3611(4)
_cell_length_b                   12.8811(6)
_cell_length_c                   14.9160(7)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.35
_cell_volume                     1733.55(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_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  0.0716
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            64128
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.195
_diffrn_reflns_theta_max         25.195
_diffrn_reflns_theta_min         2.236
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1522 before and 0.0901 after correction.
The Ratio of minimum to maximum transmission is 0.6358.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'Reddish orange'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       needle
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.544
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0372P)^2^+3.9209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4800
_reflns_number_total             6224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01022a2.cif
_cod_data_source_block           psh_115_0m
_cod_depositor_comments
;
Adding full bibliography for 7716197--7716200.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C78 H96 N2 Ni2 P4'
_cod_original_formula_weight         1302.86
_cod_original_formula_moiety         '2(C39 H48 N Ni P2)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1733.54(14)
_cod_database_code               7716197
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.686
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C28(H28), C31(H31), C37(H37), C34(H34)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C21(H21), C18(H18), C20(H20), C9(H9), C17(H17), C19(H19), C2(H2),
 C11(H11), C24(H24), C25(H25), C27(H27), C23(H23), C26(H26)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C33(H33A,H33B,H33C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C30(H30A,
 H30B,H30C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              12852
_olex2_submission_special_instructions 'No special instructions were received'