Three routes to nickel(ii) salicylaldehyde 4-phenyl and 4-methylthiosemicarbazonato complexes: mechanochemical, electrochemical and conventional approach
Cindrić, Marina; Uzelac, Marina; Cinčić, Dominik; Halasz, Ivan; Pavlović, Gordana; Hrenar, Tomica; Ćurić, Manda; Kovačević, Davor; CrystEngComm 14 (2012) 3039–; doi:10.1039/c2ce06611d

data_7207824
_publ_section_title
;
 Three routes to nickel(ii) salicylaldehyde 4-phenyl and
 4-methylthiosemicarbazonato complexes: mechanochemical, electrochemical
 and conventional approach
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              3039
_journal_paper_doi               10.1039/c2ce06611d
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C28 H24 N6 Ni O2 S2, C H4 O'
_chemical_formula_sum            'C29 H28 N6 Ni O3 S2'
_chemical_formula_weight         631.40
_chemical_name_common
;
salicylaldehyde 4-phenylthiosemicarbazone)-(salicylaldehyde
4-phenylthiosemicarbazonato)-nickel(ii) methanol (1/1) solvate
;
_chemical_name_systematic
;
(salicylaldehyde 4-phenylthiosemicarbazone)-(salicylaldehyde
4-phenylthiosemicarbazonato)-nickel(ii) methanol (1/1) solvate

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.188(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.386(2)
_cell_length_b                   18.7538(17)
_cell_length_c                   7.9689(13)
_cell_measurement_reflns_used    4758
_cell_measurement_theta_max      29.0161
_cell_measurement_theta_min      4.1544
_cell_volume                     2860.0(6)
_computing_cell_refinement
'CrysAlis RED, Oxford Diffraction Ltd.Version 1.171.34.44'
_computing_data_collection
'CrysAlis CCD, Oxford Diffraction Ltd.Version 1.171.34.44'
_computing_data_reduction
'CrysAlis RED, Oxford Diffraction Ltd.Version 1.171.34.44'
_computing_molecular_graphics
;
ORTEP-3 for Windows, Ver. 1.70.01 (Farrugia, 2005),
MERCURY 1.4.2 (CCDC, 2006)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w - scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1451
_diffrn_reflns_av_sigmaI/netI    0.1443
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16245
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.16
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5004
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1694
_refine_ls_R_factor_gt           0.0914
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+13.3209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1926
_reflns_number_gt                2976
_reflns_number_total             5004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce06611d.txt
_cod_data_source_block           exp_1863_MeOH_solvate
_cod_original_cell_volume        2860.1(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7207824