Synthesis, crystal structure and reactivity of η<sup>2</sup>-thiophyne Ni complexes.
Terada, Misaki; Nishii, Yuji; Miura, Masahiro; Chemical communications (Cambridge, England) 54 (2018) 2918–2921; doi:10.1039/c8cc00705e

data_7121313
_publ_section_title
;
 Synthesis, crystal structure and reactivity of \h<sup>2</sup>-thiophyne
 Ni complexes.
;
_journal_issue                   23
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2918
_journal_page_last               2921
_journal_paper_doi               10.1039/c8cc00705e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'0.67(C39 H62 Ni P2 S Si), 0.33(C38.93 H61.47 Ni P2 S Si)'
_chemical_formula_sum            'C38.98 H61.83 Ni P2 S Si'
_chemical_formula_weight         711.25
_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.cc1z0qmb
_audit_creation_date             2017-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                82.1370(10)
_cell_angle_beta                 82.6670(10)
_cell_angle_gamma                83.181(2)
_cell_formula_units_Z            6
_cell_length_a                   10.9627(2)
_cell_length_b                   15.9681(3)
_cell_length_c                   35.1062(4)
_cell_measurement_reflns_used    21408
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.3550
_cell_measurement_theta_min      3.8660
_cell_volume                     6005.73(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_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    -64.00  29.00   0.50    1.45    --  -42.80  37.00  90.00  186
  2  \w     -7.00  25.00   0.50    1.45    --  -42.80 100.00 141.00   64
  3  \w    -57.00 -32.00   0.50    9.45    -- -106.00  77.00 150.00   50
  4  \w    -70.00 -45.00   0.50    9.45    -- -106.00 100.00 141.00   50
  5  \w    -92.00 -58.00   0.50    9.45    -- -106.00  57.00  30.00   68
  6  \w    -61.00 -33.00   0.50    9.45    -- -106.00  57.00 -60.00   56
  7  \w    -60.00 -35.00   0.50    9.45    -- -106.00  77.00 -60.00   50
  8  \w    -68.00 -32.00   0.50    9.45    -- -106.00 125.00 -60.00   72
  9  \w    -75.00 -37.00   0.50    9.45    -- -106.00 125.00   0.00   76
 10  \w    -80.00 -33.00   0.50    9.45    -- -106.00 125.00 -90.00   94
 11  \w    -69.00 -42.00   0.50    9.45    -- -106.00 125.00-120.00   54
 12  \w    -78.00 -36.00   0.50    9.45    -- -106.00 125.00-180.00   84
 13  \w    -95.00 -25.00   0.50    1.45    --  -42.80 125.00-180.00  140
 14  \w    -99.00 -73.00   0.50    9.45    -- -106.00 125.00 -60.00   52
 15  \w   -115.00 -90.00   0.50    9.45    -- -106.00 125.00 -90.00   50
 16  \w   -103.00 -32.00   0.50    9.45    -- -106.00 125.00-150.00  142
 17  \w   -103.00 -72.00   0.50    9.45    -- -106.00  37.00 -30.00   62
 18  \w   -128.00 -80.00   0.50    9.45    -- -106.00  57.00 -60.00   96
 19  \w   -134.00 -33.00   0.50    9.45    -- -106.00  77.00  30.00  202
 20  \w    -79.00 -53.00   0.50    1.45    --  -42.80 100.00 141.00   52
 21  \w     72.00 117.00   0.50    1.45    --   42.80 125.00 -90.00   90
 22  \w     72.00 114.00   0.50    1.45    --   42.80 125.00-120.00   84
 23  \w     93.00 118.00   0.50    9.45    --   76.50 100.00 141.00   50
 24  \w    -20.00  40.00   0.50    1.45    --   42.80-100.00  36.00  120
 25  \w     32.00  57.00   0.50    9.45    --   76.50-100.00  36.00   50
 26  \w    -28.00  65.00   0.50    1.45    --   42.80 -57.00-120.00  186
 27  \w    -63.00 -38.00   0.50    1.45    --  -42.80 125.00  60.00   50
 28  \w   -106.00 -45.00   0.50    9.45    -- -106.00  37.00 150.00  122
 29  \w   -115.00 -70.00   0.50    9.45    -- -106.00 125.00 120.00   90
 30  \w   -114.00 -88.00   0.50    9.45    -- -106.00 125.00  60.00   52
 31  \w   -121.00 -83.00   0.50    9.45    -- -106.00 125.00   0.00   76
 32  \w   -126.00 -82.00   0.50    9.45    -- -106.00  77.00 -60.00   88
 33  \w   -121.00 -75.00   0.50    9.45    -- -106.00 125.00-120.00   92
 34  \w   -121.00 -96.00   0.50    9.45    -- -106.00 125.00-180.00   50
 35  \w   -127.00 -32.00   0.50    9.45    -- -106.00  57.00-180.00  190
 36  \w   -123.00 -75.00   0.50    9.45    -- -106.00 -19.00 -60.00   96
 37  \w   -139.00-113.00   0.50    9.45    -- -106.00-100.00  36.00   52
 38  \w   -166.00-118.00   0.50    9.45    -- -106.00 -57.00 150.00   96
 39  \w   -175.00-136.00   0.50    9.45    -- -106.00 -37.00  60.00   78
 40  \w   -175.00 -87.00   0.50    9.45    -- -106.00 -77.00  90.00  176
 41  \w   -101.00 -70.00   0.50    1.45    --  -42.80-125.00 150.00   62
 42  \w   -161.00 -83.00   0.50    9.45    -- -106.00 -99.00  60.00  156
 43  \w   -110.00 -82.00   0.50    1.45    --  -42.80-125.00 -90.00   56
 44  \w   -150.00 -95.00   0.50    9.45    -- -106.00 -99.00-120.00  110
 45  \w   -169.00-140.00   0.50    9.45    -- -106.00 -19.00 -60.00   58
 46  \w   -174.00 -83.00   0.50    9.45    -- -106.00 -57.00 -30.00  182
 47  \w   -135.00 -26.00   0.50    9.45    -- -106.00  19.00-150.00  218
 48  \w   -121.00 -89.00   0.50    9.45    -- -106.00 125.00  90.00   64
 49  \w   -135.00 -62.00   0.50    9.45    -- -106.00  77.00 150.00  146
 50  \w   -149.00 -92.00   0.50    9.45    -- -106.00 -77.00 120.00  114
 51  \w   -177.00-110.00   0.50    9.45    -- -106.00-125.00  60.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0270263000
_diffrn_orient_matrix_UB_12      0.0970565000
_diffrn_orient_matrix_UB_13      -0.0006376000
_diffrn_orient_matrix_UB_21      -0.0275567000
_diffrn_orient_matrix_UB_22      0.0079145000
_diffrn_orient_matrix_UB_23      -0.0423641000
_diffrn_orient_matrix_UB_31      -0.1371165000
_diffrn_orient_matrix_UB_32      -0.0102360000
_diffrn_orient_matrix_UB_33      0.0138856000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            88967
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.953
_diffrn_reflns_theta_min         3.558
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       plate
_exptl_crystal_F_000             2302
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1245
_refine_ls_number_reflns         23970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0950P)^2^+1.7221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18504
_reflns_number_total             23970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00705e2.cif
_cod_data_source_block           20171004-4
_cod_depositor_comments
'Adding full bibliography for 7121308--7121314.cif.'
_cod_database_code               7121313
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         NiP2SiSC39H62
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C03L)=Sof(H03S)=Sof(H03T)=Sof(H03U)=Sof(C03N)=Sof(H03X)=Sof(H03Y)=
 Sof(H0GA)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Sof(H01F)=Sof(C0AA)=Sof(H0AA)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(C2AA)=
 Sof(H2AA)=Sof(H2AB)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(C4AA)=Sof(H4AA)=
 Sof(H4AB)=1-FVAR(2)
 Sof(H01R)=Sof(C03H)=Sof(H03K)=Sof(H03L)=Sof(C03I)=Sof(H03M)=Sof(H03N)=
 Sof(C03J)=Sof(H03O)=Sof(H03P)=Sof(C03K)=Sof(H03Q)=Sof(H03R)=Sof(C03M)=
 Sof(H03V)=Sof(H03W)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J), C00L(H00L), C00M(H00M),
 C00N(H00N), C00P(H00P), C00S(H00S), C00V(H00V), C01R(H01R), C01R(H01F),
 C01S(H01S)
3.b Secondary CH2 refined with riding coordinates:
 C00K(H00C,H00D), C00Z(H00A,H00B), C010(H01V,H01W), C015(H01I,H01J), C018(H01K,
 H01L), C01A(H01M,H01N), C01B(H01X,H01Y), C01C(H01A,H01B), C01F(H01Z,H),
 C01H(H01,HA), C01J(H0CA,HB), C01K(H1CA,HC), C01M(H3CA,HD), C01O(H01P,H01Q),
 C01P(H01C,H01D), C01Q(H4CA,HE), C01T(H01G,H01H), C01U(H5CA,HF), C01W(H6CA,HG),
 C01X(H01T,H01U), C01Y(H7CA,HH), C01Z(H8CA,HI), C021(H02A,H02B), C022(H02C,
 H02D), C023(H02T,H02U), C024(H0DA,HL), C025(H1DA,HM), C028(H02V,H02X),
 C02B(H02Z,HN), C02C(H2DA,HO), C02D(H02,HP), C02E(H02E,H02F), C02F(H5AA,HQ),
 C02G(H6AA,HR), C02H(H3DA,HS), C02I(H7AA,HT), C02J(H02G,H02H), C02K(H02I,H02J),
 C02M(H5DA,HU), C02O(H02K,H02L), C02P(H9AA,HV), C02Q(H02M,H02N), C02T(H02O,
 H02P), C02U(H1BA,HY), C02V(H2BA,HZ), C02X(H6DA,H2EA), C02Y(H7DA,H3EA),
 C02Z(H02Q,H02R), C030(H03Z,H4EA), C031(H03A,H03B), C032(H03C,H03D), C033(H03,
 H5EA), C035(H8DA,H8EA), C036(H03E,H03F), C037(H03G,H03H), C038(H03I,H03J),
 C03B(H0EA,H3FA), C03C(H5BA,H4FA), C03D(H6BA,H5FA), C03F(H7BA,H8FA), C03G(H8BA,
 H9FA), C03H(H03K,H03L), C03I(H03M,H03N), C03J(H03O,H03P), C03K(H03Q,H03R),
 C03M(H03V,H03W), C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C3AA(H3AA,H3AB), C4AA(H4AA,
 H4AB)
3.c Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00U(H00U), C016(H016), C019(H019), C01E(H01E), C01G(H01O),
 C01I(H9BA), C01L(H2CA), C026(H026), C029(H029), C02A(H02Y), C02L(H4DA),
 C02N(H8AA), C02S(H02S), C02W(H02W), C0AA(H0AA)
3.d Idealised Me refined as rotating group:
 C020(H9CA,HJ,HK), C02R(H0BA,HW,HX), C034(H3BA,H6EA,H7EA), C039(H4BA,H9EA,
 H0FA), C03A(H9DA,H1FA,H2FA), C03E(H1EA,H6FA,H7FA), C03L(H03S,H03T,H03U),
 C03N(H03X,H03Y,H0GA), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              52678
_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 3.382
_oxdiff_exptl_absorpt_empirical_full_min 0.254