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_7701895
_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         'C43 H41 Ni P1.95 S2, C24 H20 B, 0.05(P)'
_chemical_formula_sum            'C67 H61 B Ni P2 S2'
_chemical_formula_weight         1061.73
_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.cc1zsmft
_audit_creation_date             2018-09-08
_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                91.9485(8)
_cell_angle_beta                 103.1258(10)
_cell_angle_gamma                97.6660(9)
_cell_formula_units_Z            2
_cell_length_a                   11.49513(14)
_cell_length_b                   13.94818(14)
_cell_length_c                   17.43870(17)
_cell_measurement_reflns_used    16845
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.5870
_cell_measurement_theta_min      3.9350
_cell_volume                     2692.67(5)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.932
_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    -97.00 -49.00   0.50    0.05    --  -48.45 131.00  14.00   96
  2  \w    -83.00 -58.00   0.50    0.05    --  -48.45 138.00-170.00   50
  3  \w   -100.00 -46.00   0.50    0.10    --  -86.25 138.00-170.00  108
  4  \w    -98.00 -22.00   0.50    0.10    --  -86.25 131.00  14.00  152
  5  \w     95.00 176.00   0.50    0.10    --  107.75  19.00  60.00  162
  6  \w     99.00 177.00   0.50    0.10    --  107.75  37.00  90.00  156
  7  \w    109.00 134.00   0.50    0.10    --  107.75 131.00  14.00   50
  8  \w     92.00 178.00   0.50    0.10    --  107.75 125.00 -30.00  172
  9  \w     84.00 171.00   0.50    0.10    --  107.75 138.00-170.00  174
 10  \w    -61.00  24.00   0.50    0.05    --  -48.45  37.00 150.00  170
 11  \w     35.00  60.00   0.50    0.05    --   48.45-131.00 -56.00   50
 12  \w   -118.00 -68.00   0.50    0.05    --  -48.45-138.00 128.00  100
 13  \w   -114.00 -73.00   0.50    0.05    --  -48.45-125.00 150.00   82
 14  \w   -135.00-110.00   0.50    0.10    --  -86.25-138.00 128.00   50
 15  \w   -137.00-112.00   0.50    0.10    --  -86.25-131.00 -56.00   50
 16  \w   -110.00 -75.00   0.50    0.05    --  -48.45-131.00 -56.00   70
 17  \w     35.00 121.00   0.50    0.10    --  107.75 -57.00  90.00  172
 18  \w     37.00 119.00   0.50    0.10    --  107.75 -37.00  60.00  164
 19  \w     36.00 123.00   0.50    0.10    --  107.75 -57.00 -90.00  174
 20  \w     35.00 120.00   0.50    0.10    --  107.75 -37.00-120.00  170
 21  \w     61.00 124.00   0.50    0.10    --  107.75-131.00 -56.00  126
 22  \w     68.00  93.00   0.50    0.05    --   48.45-138.00 128.00   50
 23  \w    102.00 127.00   0.50    0.10    --  107.75-138.00 128.00   50
 24  \w   -120.00 -37.00   0.50    0.05    --  -48.45 -57.00-180.00  166
 25  \w   -155.00-119.00   0.50    0.10    --  -86.25 -57.00   0.00   72
 26  \w   -109.00 -71.00   0.50    0.10    --  -86.25 -57.00   0.00   76
;
_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      -0.0071440000
_diffrn_orient_matrix_UB_12      -0.0403134000
_diffrn_orient_matrix_UB_13      -0.0845524000
_diffrn_orient_matrix_UB_21      0.0791997000
_diffrn_orient_matrix_UB_22      -0.0767159000
_diffrn_orient_matrix_UB_23      0.0333148000
_diffrn_orient_matrix_UB_31      -0.1141080000
_diffrn_orient_matrix_UB_32      -0.0704618000
_diffrn_orient_matrix_UB_33      0.0025031000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28724
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.139
_diffrn_reflns_theta_min         3.991
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43128
_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            orange
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       rod
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.43128
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0706P)^2^+2.3041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9322
_reflns_number_total             10630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03188f2.cif
_cod_data_source_block           171017zal-2
_cod_database_code               7701895
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         NiPSC
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.363
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: P1(0.95) P0AA(0.05)
 Fixed Uiso: H1A(0.047) H1B(0.047) H2(0.05) H3A(0.053) H3B(0.053) H4A(0.047)
 H4B(0.047) H5A(0.049) H5B(0.049) H6A(0.039) H6B(0.039) H7A(0.037) H7B(0.037)
 H9(0.042) H10(0.047) H11(0.048) H12(0.045) H15(0.044) H16(0.05) H17(0.056)
 H18(0.054) H19(0.048) H21(0.058) H22(0.07) H23(0.059) H24(0.056) H25(0.05)
 H27(0.04) H28(0.046) H29(0.05) H30(0.052) H31(0.043) H33(0.038) H34(0.044)
 H35(0.043) H36(0.044) H37(0.04) H40(0.038) H41(0.044) H42(0.043) H43(0.038)
 H45(0.04) H46(0.053) H47(0.057) H48(0.055) H49(0.044) H50(0.042) H51(0.051)
 H52(0.05) H53(0.047) H54(0.041) H57(0.042) H58(0.045) H59(0.048) H60(0.05)
 H61(0.043) H63(0.04) H64(0.045) H65(0.042) H66(0.043) H67(0.037)
 Fixed X: H1A(0.8598) H1B(0.7975) H2(1.0269) H3A(0.8791) H3B(0.9903)
 H4A(0.4811) H4B(0.5984) H5A(0.6005) H5B(0.5823) H6A(0.6113) H6B(0.5905)
 H7A(0.7683) H7B(0.8807) H9(0.2282) H10(0.1093) H11(0.193) H12(0.3942)
 H15(0.2824) H16(0.2103) H17(0.2918) H18(0.4473) H19(0.5179) H21(0.2561)
 H22(0.1825) H23(0.2804) H24(0.4503) H25(0.5275) H27(0.7198) H28(0.7237)
 H29(0.889) H30(1.0447) H31(1.0384) H33(1.1047) H34(1.2902) H35(1.3094)
 H36(1.143) H37(0.9572) H40(0.7039) H41(0.5454) H42(0.4993) H43(0.6112)
 H45(0.1899) H46(0.2489) H47(0.3387) H48(0.3619) H49(0.3014) H50(0.4422)
 H51(0.6068) H52(0.5871) H53(0.3977) H54(0.2335) H57(0.052) H58(-0.0986) H59(-
 0.1642) H60(-0.074) H61(0.0803) H63(-0.0229) H64(-0.0788) H65(0.06)
 H66(0.2583) H67(0.3141)
 Fixed Y: H1A(0.4638) H1B(0.478) H2(0.5735) H3A(0.6354) H3B(0.7058)
 H4A(0.5293) H4B(0.4841) H5A(0.5228) H5B(0.6296) H6A(0.6084) H6B(0.5109)
 H7A(0.7056) H7B(0.7501) H9(0.6604) H10(0.5174) H11(0.4038) H12(0.4315)
 H15(0.8654) H16(0.8869) H17(0.8145) H18(0.7242) H19(0.7029) H21(0.7475)
 H22(0.8591) H23(1.0173) H24(1.063) H25(0.9514) H27(0.8185) H28(0.9118)
 H29(1.0278) H30(1.0562) H31(0.9673) H33(0.7464) H34(0.8157) H35(0.9631)
 H36(1.0415) H37(0.9733) H40(0.9487) H41(0.9863) H42(0.907) H43(0.7913)
 H45(0.4603) H46(0.6223) H47(0.7205) H48(0.6526) H49(0.4897) H50(0.3998)
 H51(0.3212) H52(0.1538) H53(0.0663) H54(0.1445) H57(0.1699) H58(0.1391)
 H59(0.2651) H60(0.4226) H61(0.4527) H63(0.3028) H64(0.2483) H65(0.1965)
 H66(0.2005) H67(0.2547)
 Fixed Z: H1A(0.7728) H1B(0.6811) H2(0.7607) H3A(0.6231) H3B(0.6816)
 H4A(0.7563) H4B(0.7535) H5A(0.8833) H5B(0.8645) H6A(0.5733) H6B(0.6132)
 H7A(0.9839) H7B(0.9538) H9(0.4505) H10(0.4631) H11(0.5439) H12(0.6061)
 H15(0.4312) H16(0.2986) H17(0.2048) H18(0.2441) H19(0.3756) H21(0.5928)
 H22(0.6622) H23(0.6877) H24(0.6412) H25(0.5741) H27(0.6371) H28(0.5299)
 H29(0.5322) H30(0.6431) H31(0.7529) H33(0.8372) H34(0.9149) H35(0.9845)
 H36(0.9779) H37(0.9004) H40(0.7581) H41(0.8091) H42(0.9146) H43(0.9704)
 H45(0.6887) H46(0.6816) H47(0.7955) H48(0.9165) H49(0.9232) H50(0.8921)
 H51(0.9363) H52(0.9257) H53(0.8735) H54(0.8305) H57(0.8354) H58(0.9019)
 H59(0.9624) H60(0.9564) H61(0.8927) H63(0.6979) H64(0.567) H65(0.5037)
 H66(0.5746) H67(0.705)
;
_shelx_res_checksum              24742
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.521