Nickel Complexes of Ligands Derived from (o-Hydroxyphenyl) Dichalcogenide: Delocalised Redox States of Nickel and o-Chalcogenophenolate Ligand
Banerjee, Sridhar; Sheet, Debobrata; Sarkar, Subhash; Halder, Partha; Paine, Tapan Kanti; Dalton Transactions  (2019) –; doi:10.1039/C9DT03413G

data_7701438
_publ_section_title
;
 Nickel Complexes of Ligands Derived from (o-Hydroxyphenyl)
 Dichalcogenide: Delocalised Redox States of Nickel and
 o-Chalcogenophenolate Ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03413G
_journal_year                    2019
_chemical_formula_moiety
'2(C28 H40 Ni O2 S2), C16 H34 N, C4 H8 O, C16 H36 N'
_chemical_formula_sum            'C92 H158 N2 Ni2 O5 S4'
_chemical_formula_weight         1617.85
_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     direct
_audit_creation_date             2019-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-24 deposited with the CCDC.    2019-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                102.301(3)
_cell_angle_beta                 96.756(3)
_cell_angle_gamma                103.944(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7642(12)
_cell_length_b                   17.6359(15)
_cell_length_c                   24.949(2)
_cell_measurement_reflns_used    8469
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.25
_cell_volume                     4829.8(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_measured_fraction_theta_full 0.749
_diffrn_measured_fraction_theta_max 0.728
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_Laue_measured_fraction_full 0.749
_diffrn_reflns_Laue_measured_fraction_max 0.728
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13155
_diffrn_reflns_point_group_measured_fraction_full 0.749
_diffrn_reflns_point_group_measured_fraction_max 0.728
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.088
_diffrn_reflns_theta_min         2.252
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.745489
_exptl_absorpt_correction_T_min  0.745489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 22103 reflections, Rint = 0.0729
 (11551 with I > 3sig(I), Rint = 0.0669)
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       needle
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         13155
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0893
_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^)+(0.0865P)^2^+26.3195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9682
_reflns_number_total             13155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03413g2.cif
_cod_data_source_block           mo_tkp060418
_cod_database_code               7701438
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7415(16)
 0.2585(16)
2. 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
3. Restrained distances
 C02S-C02T
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C02U) = Uanis(C025)
5.a Secondary CH2 refined with riding coordinates:
 C013(H6BA,HB), C01B(H7BA,HE), C01F(H8BA,HJ), C01P(H9BA,HM), C01S(H0CA,HP),
 C01U(H1CA,HQ), C01V(H6AA,HR), C01X(H2CA,HU), C024(H02S,H02T), C028(H5CA,H6DA),
 C029(H6CA,H7DA), C02A(H7CA,H8DA), C02C(H02U,H02V), C02D(H02W,H02X), C02G(H02Y,
 H1EA), C02H(H02Z,H2EA), C02I(H02,H3EA), C02J(H7AA,H4EA), C02N(H9AA,H9EA),
 C02O(H0BA,H0FA), C02R(H2BA,H5FA), C02S(H3BA,H6FA)
5.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00K(H00K), C00N(H00N), C00O(H00O), C00S(H00S), C00W(H00W),
 C00X(H00X), C010(H010), C025(H025), C02L(H1DA), C02U(H0DA), C2(H2)
5.c Idealised Me refined as rotating group:
 C00Z(H00A,H00B,H00C), C012(H01Y,H,HA), C015(H01A,H01B,H01C), C01A(H01Z,HC,HD),
  C01C(H01,HF,HG), C01E(H0AA,HH,HI), C01I(H01D,H01E,H01F), C01J(H01G,H01H,H01I),
  C01K(H1AA,HK,HL), C01L(H01J,H01K,H01L), C01M(H01M,H01N,H01O), C01N(H01P,H01Q,
 H01R), C01Q(H01S,H01T,H01U), C01R(H2AA,HN,HO), C01T(H01V,H01W,H01X), C01W(H3AA,
 HS,HT), C01Y(H4AA,HV,HW), C01Z(H5AA,HX,HY), C020(H02A,H02B,H02C), C021(H02J,
 H02K,H02L), C022(H02D,H02E,H02F), C023(H3CA,HZ,H3DA), C026(H4CA,H4DA,H5DA),
 C027(H02M,H02N,H02O), C02B(H02P,H02Q,H02R), C02E(H8CA,H9DA,H0EA), C02F(H02G,
 H02H,H02I), C02K(H8AA,H5EA,H6EA), C02M(H2DA,H7EA,H8EA), C02P(H9CA,H1FA,H2FA),
 C02Q(H1BA,H3FA,H4FA), C02T(H4BA,H7FA,H8FA), C02V(H5BA,H9FA,H0GA), C1(H1A,H1B,
 H1C)
;
_shelx_res_checksum              35032
_olex2_submission_special_instructions 'No special instructions were received'