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_7701437
_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         'C28 H40 Ni O2 Se2, C16 H36 N'
_chemical_formula_sum            'C44 H76 N Ni O2 Se2'
_chemical_formula_weight         867.68
_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             2019-09-11
_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                102.464(3)
_cell_angle_beta                 92.731(3)
_cell_angle_gamma                101.164(3)
_cell_formula_units_Z            4
_cell_length_a                   12.2167(9)
_cell_length_b                   17.5848(13)
_cell_length_c                   22.4459(17)
_cell_measurement_reflns_used    4086
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      1.21
_cell_measurement_theta_min      22.850
_cell_volume                     4599.1(6)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_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      293.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42950
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        22.847
_diffrn_reflns_theta_max         22.847
_diffrn_reflns_theta_min         1.213
_exptl_absorpt_coefficient_mu    2.038
_exptl_absorpt_correction_T_max  0.8875
_exptl_absorpt_correction_T_min  0.750971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2004/1 (Bruker,2004) was used for absorption correction. R(int) was 0.0803 before and 0.0485 after correction. The Ratio of minimum to maximum transmission is 0.7510. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         12543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+4.6140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8169
_reflns_number_total             12543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03413g2.cif
_cod_data_source_block           ds11_0m
_cod_database_code               7701437
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.792
_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.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C39(H39A,H39B), C37(H37A,H37B), C38(H38A,H38B), C29(H29A,
 H29B), C35(H35A,H35B), C33(H33A,H33B), C34(H34A,H34B), C30(H30A,H30B),
 C42(H42A,H42B), C43(H43A,H43B), C31(H31A,H31B), C81(H81A,H81B), C82(H82A,H82B),
  C85(H85A,H85B), C83(H83A,H83B), C79(H79A,H79B), C77(H77A,H77B), C78(H78A,
 H78B), C74(H74A,H74B), C75(H75A,H75B), C73(H73A,H73B), C87(H87A,H87B),
 C86(H86A,H86B)
2.b Aromatic/amide H refined with riding coordinates:
 C47(H47), C49(H49), C12(H12), C10(H10), C53(H53), C55(H55), C6(H6), C4(H4)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C44(H44A,H44B,H44C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C72(H72A,
 H72B,H72C), C66(H66A,H66B,H66C), C71(H71A,H71B,H71C), C62(H62A,H62B,H62C),
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C80(H80A,H80B,
 H80C), C88(H88A,H88B,H88C), C84(H84A,H84B,H84C), C64(H64A,H64B,H64C), C63(H63A,
 H63B,H63C), C76(H76A,H76B,H76C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              34772
_olex2_submission_special_instructions 'No special instructions were received'