Synthesis of a labile sulfur-centred ligand, [S(H)C(PPh2S)2](-): structural diversity in lithium(i), zinc(ii) and nickel(ii) complexes.
Thirumoorthi, Ramalingam; Chivers, Tristram; Häggman, Susanna; Mansikkamäki, Akseli; Morgan, Ian S.; Tuononen, Heikki M.; Lahtinen, Manu; Konu, Jari; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12691–12701; doi:10.1039/c6dt02565j

data_7039938
_publ_section_title
;
 Synthesis of a labile sulfur-centred ligand, [S(H)C(PPh2S)2](-):
 structural diversity in lithium(i), zinc(ii) and nickel(ii) complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12691
_journal_page_last               12701
_journal_paper_doi               10.1039/c6dt02565j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C50 H42 Ni1 P4 S6, 2(C7 H8)'
_chemical_formula_sum            'C64 H58 Ni P4 S6'
_chemical_formula_weight         1202.05
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-15 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.000
_cell_angle_beta                 106.2620(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   11.0600(3)
_cell_length_b                   15.7060(4)
_cell_length_c                   16.8660(4)
_cell_measurement_reflns_used    22121
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      1.8
_cell_volume                     2812.55(12)
_computing_cell_refinement       'DENZO (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 1999)'
_computing_data_reduction        'Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'phi\omega scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Enraf Nonius FR590D,fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21124
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.9118
_exptl_absorpt_correction_T_min  0.8342
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+6.3308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                5176
_reflns_number_total             6131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02565j2.cif
_cod_data_source_block           compound_4a
_cod_depositor_comments
'Adding full bibliography for 7039937--7039940.cif.'
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7039938