A new example of intra-molecular C-H⋯Ni anagostic inter-actions: synthesis, crystal structure and Hirshfeld analysis of <i>cis</i>-bis-[4-methyl-2-(1,2,3,4-tetra-hydro-naphthalen-1-yl-idene)hydrazinecarbo-thio-amidato-κ<sup>2</sup><i>N</i><sup>1</sup>,<i>S</i>]nickel(II) di-methyl-formamide monosolvate.
de Oliveira, Adriano Bof; Beck, Johannes; Mellone, Sônia Elizabeth Brown S; Daniels, Jörg; Acta crystallographica. Section E, Crystallographic communications 73 (2017) 859–863; doi:10.1107/S2056989017007198

data_2311378
_publ_section_title
;
 A new example of intra-molecular C-H&#x22EF;Ni anagostic inter-actions:
 synthesis, crystal structure and Hirshfeld analysis of
 <i>cis</i>-bis-[4-methyl-2-(1,2,3,4-tetra-hydro-naphthalen-1-yl-idene)hydrazinecarbo-thio-amidato-\k<sup>2</sup><i>N</i><sup>1</sup>,<i>S</i>]nickel(II)
 di-methyl-formamide monosolvate.
;
_journal_coeditor_code           WM5389
_journal_issue                   'Pt 6'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              859
_journal_page_last               863
_journal_paper_doi               10.1107/S2056989017007198
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Ni (C12 H14 N3 S1)2], C3 H7 N O'
_chemical_formula_moiety         'C24 H28 N6 Ni S2, C3 H7 N O'
_chemical_formula_sum            'C27 H35 N7 Ni O S2'
_chemical_formula_weight         596.45
_chemical_name_systematic
;<i>cis</i>-Bis[4-methyl-2-(1,2,3,4-tetrahydronaphthalen-1-ylidene)hydrazinecarbothioamidato-\k^2^<i>N</i>^1^,<i>S</i>]nickel(II)
dimethylformamide monosolvate
;
_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_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.5290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5864(3)
_cell_length_b                   11.6273(3)
_cell_length_c                   19.1271(5)
_cell_measurement_reflns_used    105836
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     2799.05(12)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006) and <i>Crystal Explorer</i> (Wolff <i>et
al.</i>,
2012)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010) and <i>enCIFer</i> (Allen <i>et al.</i>,
2004)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015) and WinGX (Farrugia, 2012)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46078
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.458
_diffrn_reflns_theta_min         3.188
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.9810
_exptl_absorpt_correction_T_min  0.7613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0352P)^2^+1.1854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                4870
_reflns_number_total             6368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5389sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2311378
_shelx_estimated_absorpt_t_min   0.761
_shelx_estimated_absorpt_t_max   0.981
_shelx_hkl_checksum              43547
_shelx_res_checksum              87132