Reactivity of the diphosphinodithio ligated nickel(0) complex toward alkyl halides and resultant nickel(i) and nickel(ii)-alkyl complexes.
Zhang, Ailing; Wang, Congxiao; Lai, Xiaoyu; Zhai, Xiaofang; Pang, Maofu; Tung, Chen-Ho; Wang, Wenguang; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15757–15764; doi:10.1039/c8dt03188f

data_7701894
_publ_section_title
;
 Reactivity of the diphosphinodithio ligated nickel(0) complex toward
 alkyl halides and resultant nickel(i) and nickel(ii)-alkyl complexes.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15757
_journal_page_last               15764
_journal_paper_doi               10.1039/c8dt03188f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C40 H36 Ni P2 S2, C4 H8 O'
_chemical_formula_sum            'C44 H44 Ni O P2 S2'
_chemical_formula_weight         773.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc1zsmcr
_audit_creation_date             2018-09-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-08 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                85.898(2)
_cell_angle_beta                 86.077(2)
_cell_angle_gamma                80.810(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5713(3)
_cell_length_b                   13.7242(5)
_cell_length_c                   14.7211(3)
_cell_measurement_reflns_used    10265
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.3160
_cell_measurement_theta_min      4.2630
_cell_volume                     1900.84(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    -24.00  14.00   1.00    0.10    --   48.45 -20.00 164.00   38
  2  \w     33.00  59.00   1.00    0.10    --   48.45 -20.00 164.00   26
  3  \w     56.00 120.00   1.00    0.10    --   48.45  20.00 -28.00   64
  4  \w    -43.00 -14.00   1.00    0.20    --  -86.25  20.00 -28.00   29
  5  \w   -160.00-134.00   1.00    0.20    --  -86.25 -20.00 164.00   26
  6  \w   -130.00 -77.00   1.00    0.20    --  -86.25 -20.00 164.00   53
  7  \w    104.00 177.00   1.00    0.20    --  107.75  20.00 -28.00   73
  8  \w     38.00 119.00   1.00    0.20    --  107.75 -20.00 164.00   81
  9  \w    -43.00  -8.00   1.00    0.10    --  -48.45  20.00 -28.00   35
 10  \w   -118.00 -36.00   1.00    0.10    --  -48.45 -20.00 164.00   82
 11  \w    -24.00  61.00   1.00    0.10    --   48.45 -37.00  30.00   85
 12  \w    -23.00  14.00   1.00    0.10    --   48.45 -57.00 -60.00   37
 13  \w     18.00  63.00   1.00    0.10    --   48.45 -57.00 -60.00   45
 14  \w   -100.00 -17.00   1.00    0.20    --  -86.25  57.00-180.00   83
 15  \w     49.00 104.00   1.00    0.20    --  107.75 -99.00 150.00   55
 16  \w     35.00 121.00   1.00    0.20    --  107.75 -57.00 -90.00   86
 17  \w     40.00 108.00   1.00    0.20    --  107.75 -99.00  60.00   68
 18  \w     38.00 112.00   1.00    0.20    --  107.75 -37.00  30.00   74
 19  \w     37.00 115.00   1.00    0.20    --  107.75-125.00  60.00   78
 20  \w     40.00 128.00   1.00    0.20    --  107.75 -77.00-150.00   88
 21  \w     96.00 178.00   1.00    0.20    --  107.75  19.00  60.00   82
 22  \w     36.00 109.00   1.00    0.20    --  107.75 -99.00-150.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0384576000
_diffrn_orient_matrix_UB_12      -0.1051811000
_diffrn_orient_matrix_UB_13      0.0107019000
_diffrn_orient_matrix_UB_21      0.1522369000
_diffrn_orient_matrix_UB_22      -0.0413128000
_diffrn_orient_matrix_UB_23      0.0260634000
_diffrn_orient_matrix_UB_31      -0.0449371000
_diffrn_orient_matrix_UB_32      0.0144755000
_diffrn_orient_matrix_UB_33      0.1012480000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17621
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.072
_diffrn_reflns_theta_max         67.072
_diffrn_reflns_theta_min         4.310
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0359P)^2^+1.2075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5761
_reflns_number_total             6728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03188f2.cif
_cod_data_source_block           171225zal-1
_cod_original_cell_volume        1900.83(9)
_cod_database_code               7701894
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         NiPSC
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: C0AA(0.5) H0AA(0.5) H0AB(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5)
 H3AA(0.5) H3AB(0.5) H3AC(0.5) H3AD(0.5) C4AA(0.5) H4AA(0.5) H4AB(0.5)
 C5AA(0.5) H5AA(0.5) H5AB(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C0AA(H0AA,H0AB),
 C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C3AA(H3AA,H3AB), C3AA(H3AC,H3AD), C4AA(H4AA,
 H4AB), C5AA(H5AA,H5AB)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C37(H37), C38(H38), C39(H39), C40(H40)
;
_shelx_res_checksum              85842
_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 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.777