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_7039940
_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 P4 S6 Zn'
_chemical_formula_sum            'C50 H42 P4 S6 Zn'
_chemical_formula_weight         1024.44
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Hygroscopic'
_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             2016-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-06-27 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7455(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.72456(17)
_cell_length_b                   18.3260(3)
_cell_length_c                   11.6699(2)
_cell_measurement_reflns_used    4394
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.3830
_cell_measurement_theta_min      4.4630
_cell_volume                     2288.68(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'SIR2008 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -70.00 -35.00   1.00    1.50    --  -41.65  77.00 -30.00   35
  2  \w    -91.00 -17.00   1.00    1.50    --  -41.65 -57.00  60.00   74
  3  \w   -113.00 -16.00   1.00    1.50    --  -41.65 -57.00 -30.00   97
  4  \w     50.00  86.00   1.00    6.00    --  112.00 -94.00-180.00   36
  5  \w     42.00 108.00   1.00    6.00    --  112.00 -94.00 -60.00   66
  6  \w     84.00 174.00   1.00    6.00    --  112.00  30.00 120.00   90
  7  \w     44.00 130.00   1.00    6.00    --  112.00 -30.00 150.00   86
  8  \w     86.00 178.00   1.00    6.00    --  112.00  30.00-150.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0898172000
_diffrn_orient_matrix_UB_12      -0.0005087000
_diffrn_orient_matrix_UB_13      0.1085080000
_diffrn_orient_matrix_UB_21      0.1040878000
_diffrn_orient_matrix_UB_22      -0.0317260000
_diffrn_orient_matrix_UB_23      -0.0701700000
_diffrn_orient_matrix_UB_31      0.0429603000
_diffrn_orient_matrix_UB_32      0.0778391000
_diffrn_orient_matrix_UB_33      -0.0280311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7806
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.952
_diffrn_reflns_theta_min         4.131
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.907
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.409
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.487
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.037
_refine_diff_density_min         -2.700
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0366P)^2^+8.1524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4025
_reflns_number_total             4641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02565j2.cif
_cod_data_source_block           jk1605_a
_cod_depositor_comments
'Adding full bibliography for 7039937--7039940.cif.'
_cod_original_cell_volume        2288.69(7)
_cod_database_code               7039940
_chemical_oxdiff_formula         'C50 H42 P4 S6 Zn1'
_chemical_oxdiff_usercomment     'colorless plate'
_reflns_odcompleteness_completeness 99.53
_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:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              17768
_shelx_shelxl_version_number     2014/7
_ins_header
;
TITL jk1605_a in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  10.724557  18.326010  11.669916  90.0000  93.7455  90.0000
ZERR    2.00   0.000173   0.000346   0.000206   0.0000   0.0016   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H P S Zn
UNIT 100.00 84.00 8.00 12.00 2.00
TREF
HKLF 4
END
;
_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 1.382
_oxdiff_exptl_absorpt_empirical_full_min 0.665
_solvent_exptl_crystal_recrystallization_method 'CH2Cl2, Et2O'