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_7701896
_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, C24 H20 B'
_chemical_formula_sum            'C64 H56 B Ni P2 S2'
_chemical_formula_weight         1020.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1zsmds
_audit_creation_date             2018-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-10-08 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6906(3)
_cell_length_b                   21.6675(3)
_cell_length_c                   27.8121(4)
_cell_measurement_reflns_used    14136
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.5070
_cell_measurement_theta_min      4.3930
_cell_volume                     11263.3(3)
_computing_data_collection       '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, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34031
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.504
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61167
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       rod
_exptl_crystal_F_000             4280
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;

;
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+7.0034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8149
_reflns_number_total             9960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03188f2.cif
_cod_data_source_block           180403zal-1_sq
_cod_original_cell_volume        11263.4(3)
_cod_database_code               7701896
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   1.00000
_shelx_estimated_absorpt_t_min   0.61167
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.059) H1B(0.059) H2A(0.059) H2B(0.059) H3A(0.049) H3B(0.049)
 H4A(0.052) H4B(0.052) H7(0.054) H8(0.06) H9(0.059) H10(0.048) H12(0.055)
 H13(0.073) H14(0.076) H15(0.07) H16(0.056) H18(0.059) H19(0.084) H20(0.089)
 H21(0.09) H22(0.069) H25(0.043) H26(0.049) H27(0.052) H28(0.049) H30(0.054)
 H31(0.062) H32(0.05) H33(0.046) H34(0.039) H36(0.051) H37(0.064) H38(0.058)
 H39(0.054) H40(0.049) H42(0.067) H43(0.085) H44(0.078) H45(0.061) H46(0.047)
 H48(0.056) H49(0.072) H50(0.082) H51(0.079) H52(0.057) H54(0.051) H55(0.058)
 H56(0.059) H57(0.056) H58(0.043) H60(0.043) H61(0.052) H62(0.059) H63(0.06)
 H64(0.052)
 Fixed X: H1A(0.3715) H1B(0.4407) H2A(0.375) H2B(0.3702) H3A(0.3623)
 H3B(0.4206) H4A(0.1774) H4B(0.2425) H7(0.2997) H8(0.3353) H9(0.3108)
 H10(0.2549) H12(0.1065) H13(-0.0166) H14(-0.0907) H15(-0.0418) H16(0.0801)
 H18(0.1272) H19(0.1623) H20(0.2784) H21(0.3628) H22(0.3286) H25(0.1571)
 H26(0.2104) H27(0.3331) H28(0.4028) H30(0.0998) H31(-0.02) H32(-0.0841) H33(-
 0.0273) H34(0.0937) H36(0.2156) H37(0.2454) H38(0.2759) H39(0.2746)
 H40(0.2436) H42(0.5519) H43(0.5125) H44(0.4985) H45(0.5198) H46(0.5592)
 H48(0.7084) H49(0.8301) H50(0.8832) H51(0.8124) H52(0.6906) H54(0.4561)
 H55(0.3971) H56(0.4612) H57(0.5851) H58(0.6439) H60(0.5339) H61(0.5278)
 H62(0.5718) H63(0.6269) H64(0.6352)
 Fixed Y: H1A(0.2501) H1B(0.2808) H2A(0.3129) H2B(0.2406) H3A(0.3779)
 H3B(0.3283) H4A(0.3062) H4B(0.2712) H7(0.3209) H8(0.4087) H9(0.5048)
 H10(0.5132) H12(0.4196) H13(0.4209) H14(0.4369) H15(0.4515) H16(0.4462)
 H18(0.5506) H19(0.6469) H20(0.6657) H21(0.589) H22(0.4915) H25(0.2536)
 H26(0.1688) H27(0.1574) H28(0.233) H30(0.2988) H31(0.2763) H32(0.3138)
 H33(0.3718) H34(0.393) H36(0.4921) H37(0.5742) H38(0.5578) H39(0.4596)
 H40(0.3768) H42(0.0995) H43(0.0972) H44(0.1878) H45(0.2811) H46(0.2832)
 H48(0.2153) H49(0.2012) H50(0.1566) H51(0.126) H52(0.1387) H54(0.1585)
 H55(0.0776) H56(-0.0022) H57(0.001) H58(0.083) H60(0.2168) H61(0.3038)
 H62(0.397) H63(0.3998) H64(0.3122)
 Fixed Z: H1A(0.6471) H1B(0.6686) H2A(0.7365) H2B(0.7314) H3A(0.5582)
 H3B(0.5696) H4A(0.7691) H4B(0.7913) H7(0.8494) H8(0.8898) H9(0.8585)
 H10(0.7848) H12(0.7954) H13(0.8052) H14(0.7401) H15(0.6644) H16(0.6539)
 H18(0.7014) H19(0.6738) H20(0.653) H21(0.6608) H22(0.685) H25(0.5357)
 H26(0.5009) H27(0.5036) H28(0.5382) H30(0.6404) H31(0.6325) H32(0.5679)
 H33(0.5098) H34(0.5164) H36(0.596) H37(0.5471) H38(0.4677) H39(0.4369)
 H40(0.4852) H42(0.6992) H43(0.777) H44(0.8197) H45(0.782) H46(0.7037)
 H48(0.5755) H49(0.5778) H50(0.6447) H51(0.7082) H52(0.7056) H54(0.6212)
 H55(0.5857) H56(0.5508) H57(0.5518) H58(0.5869) H60(0.5474) H61(0.5008)
 H62(0.529) H63(0.6038) H64(0.6493)
;
_shelx_res_checksum              74270
_shelx_fab_checksum              31882
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'