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_7716917
_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         'C80 H122 N6 Ni2 O4 P2 S4, 2(B F4)'
_chemical_formula_sum            'C80 H122 B2 F8 N6 Ni2 O4 P2 S4'
_chemical_formula_weight         1713.05
_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             2024-04-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.782(4)
_cell_angle_beta                 106.703(4)
_cell_angle_gamma                96.437(5)
_cell_formula_units_Z            1
_cell_length_a                   13.0354(7)
_cell_length_b                   13.3201(7)
_cell_length_c                   14.2399(5)
_cell_measurement_reflns_used    5736
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1400
_cell_measurement_theta_min      2.4910
_cell_volume                     2350.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -85.00 -12.00   1.00   12.18    --  -10.48 -37.00   0.00   73
  2  \w    -19.00  35.00   1.00   12.18    --  -10.48  39.00 129.00   54
  3  \w    -13.00  29.00   1.00   12.18    --  -10.48 -99.00  30.00   42
  4  \w    -65.00   4.00   1.00   12.18    --  -10.48 -37.00 -90.00   69
  5  \w    -38.00  23.00   1.00   12.18    --  -10.48  57.00-180.00   61
  6  \w     44.00  96.00   1.00   12.18    --   12.36 178.00 -30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0563085000
_diffrn_orient_matrix_UB_12      -0.0159239000
_diffrn_orient_matrix_UB_13      -0.0150406000
_diffrn_orient_matrix_UB_21      0.0091513000
_diffrn_orient_matrix_UB_22      -0.0457246000
_diffrn_orient_matrix_UB_23      -0.0206384000
_diffrn_orient_matrix_UB_31      0.0045951000
_diffrn_orient_matrix_UB_32      -0.0231099000
_diffrn_orient_matrix_UB_33      0.0453723000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22453
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.565
_diffrn_reflns_theta_min         2.094
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.155
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         11134
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1724P)^2^+1.0602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2553
_refine_ls_wR_factor_ref         0.3134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6016
_reflns_number_total             11134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01915f2.cif
_cod_data_source_block           dm857c
_cod_depositor_comments
'Adding full bibliography for 7716902--7716918.cif.'
_cod_database_code               7716917
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C106  H132  B2  O4  F8  P2  S4  Ni2  N1  '
_chemical_oxdiff_usercomment     'yellow chunk'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61, C62, C63, C64, C65, C66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
C51 \\sim O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C27) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C51) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C28, C48, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C55, C54, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61, C66, C62
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C46, C27, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C51, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C27(H27), C28(H28), C51(H51), C61(H61)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C56(H56A,H56B), C62(H62A,H62B), C63(H63A,H63B),
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
5.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67593
_shelx_hkl_checksum              83677
_shelx_fab_checksum              62864
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.456
_oxdiff_exptl_absorpt_empirical_full_min 0.796