Synthesis and reactivity of air stable Ni(II) complexes with isocyanides and dialkyldithiophosphate ligands: acyclic diaminocarbene formation.
Álvarez-Miguel, Lucía; Del Carmen-Rodríguez, Clara; Valle, María; Álvarez, Celedonio M; Martín-Álvarez, José M; García-Rodríguez, Raúl; Miguel, Daniel; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15101–15112; doi:10.1039/d4dt01915f

data_7716903
_publ_section_title
;
 Synthesis and reactivity of air stable Ni(II) complexes with isocyanides
 and dialkyldithiophosphate ligands: acyclic diaminocarbene formation.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15101
_journal_page_last               15112
_journal_paper_doi               10.1039/d4dt01915f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C20 H24 N2 Ni O2 P S2, Cl O4'
_chemical_formula_sum            'C20 H24 Cl N2 Ni O6 P S2'
_chemical_formula_weight         577.66
_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     iterative
_audit_creation_date             2016-10-15
_audit_creation_method
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Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
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_audit_update_record
;
2023-10-03 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                99.859(5)
_cell_angle_beta                 97.908(4)
_cell_angle_gamma                105.106(5)
_cell_formula_units_Z            2
_cell_length_a                   7.2158(3)
_cell_length_b                   10.0031(8)
_cell_length_c                   18.9825(10)
_cell_measurement_reflns_used    3689
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.7383
_cell_measurement_theta_min      2.1557
_cell_volume                     1279.15(14)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_details
;
  1 omega  -58.00   35.00   1.0000   47.5900
omega____ theta____ kappa____ phi______ frames
    -       11.7464  -57.0000   60.0000 93

  2 omega  -12.00   68.00   1.0000   47.5900
omega____ theta____ kappa____ phi______ frames
    -       11.7464   72.0000  -26.0000 80

  3 omega  -13.00   82.00   1.0000   47.5900
omega____ theta____ kappa____ phi______ frames
    -       11.7464   57.0000 -150.0000 95
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0608961000
_diffrn_orient_matrix_UB_12      0.0453127000
_diffrn_orient_matrix_UB_13      -0.0008070000
_diffrn_orient_matrix_UB_21      0.0345658000
_diffrn_orient_matrix_UB_22      0.0209515000
_diffrn_orient_matrix_UB_23      -0.0308120000
_diffrn_orient_matrix_UB_31      -0.0765390000
_diffrn_orient_matrix_UB_32      -0.0562802000
_diffrn_orient_matrix_UB_33      -0.0233054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9842
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.804
_diffrn_reflns_theta_min         2.160
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.2747
_exptl_crystal_size_min          0.0631
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0819P)^2^+0.8576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3907
_reflns_number_total             5964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01915f2.cif
_cod_data_source_block           mv40a
_cod_depositor_comments
'Adding full bibliography for 7716902--7716918.cif.'
_cod_original_cell_volume        1279.16(13)
_cod_database_code               7716903
_chemical_oxdiff_formula         'C40 H48 N4 O8 P2 S4 Cl2 Ni2'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              37748
_shelx_hkl_checksum              57225
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'