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_7039937
_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 Li2 P4 S6'
_chemical_formula_sum            'C50 H42 Li2 P4 S6'
_chemical_formula_weight         972.95
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-09-15 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0727(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.69567(12)
_cell_length_b                   18.19940(19)
_cell_length_c                   11.90927(11)
_cell_measurement_reflns_used    7266
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.1950
_cell_measurement_theta_min      4.4150
_cell_volume                     2312.34(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000  -90.0000 82

  2 omega  -82.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   19.0000 -150.0000 121

  3 omega   23.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676 -125.0000 -120.0000 74

  4 omega   36.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 55

  5 omega   57.00  151.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000 -180.0000 94

  6 omega   84.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000   30.0000 94

  7 omega   36.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 55

  8 omega   36.00  116.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -60.0000 80

  9 omega   39.00   99.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 60

 10 omega -115.00  -13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -57.0000  150.0000 102

 11 omega -118.00   -9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -77.0000  -90.0000 109

 12 omega    9.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676   77.0000   90.0000 109

 13 omega   86.00  132.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   90.0000 46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0250334000
_diffrn_orient_matrix_UB_12      0.0817532000
_diffrn_orient_matrix_UB_13      0.0234100000
_diffrn_orient_matrix_UB_21      0.0055251000
_diffrn_orient_matrix_UB_22      -0.0159184000
_diffrn_orient_matrix_UB_23      0.1272960000
_diffrn_orient_matrix_UB_31      0.1421148000
_diffrn_orient_matrix_UB_32      0.0149932000
_diffrn_orient_matrix_UB_33      0.0084729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12842
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.989
_diffrn_reflns_theta_min         4.144
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.314
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.0862
_exptl_crystal_size_mid          0.0582
_exptl_crystal_size_min          0.0311
_refine_diff_density_max         1.548
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0511P)^2^+1.5445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3645
_reflns_number_total             4108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02565j2.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
'Adding full bibliography for 7039937--7039940.cif.'
_cod_database_code               7039937
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C50 H42 S6 P4 Li1'
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C22(H22), C21(H21), C16(H16), C8(H8), C20(H20), C11(H11), C24(H24),
 C9(H9), C12(H12), C10(H10), C3(H3), C15(H15), C17(H17), C6(H6), C2(H2),
 C18(H18), C4(H4), C5(H5), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'