Isomerism and reactivity of nickel(ii) acetylacetonate bis(thiosemicarbazone) complexes.
Bilyj, Jessica K.; Riley, Mark J.; Bernhardt, Paul V.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2018–2030; doi:10.1039/c7dt04337f

data_7045277
_publ_section_title
;
 Isomerism and reactivity of nickel(ii) acetylacetonate
 bis(thiosemicarbazone) complexes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2018
_journal_page_last               2030
_journal_paper_doi               10.1039/c7dt04337f
_journal_volume                  47
_journal_year                    2018
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C19 H18 N6 Ni1 O1 S2,C3 H7 N O'
_chemical_formula_sum            'C22 H25 N7 Ni O2 S2'
_chemical_formula_weight         542.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2017-10-21T16:08:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-10-21 deposited with the CCDC.
2018-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.341(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8455(9)
_cell_length_b                   7.4159(6)
_cell_length_c                   36.322(2)
_cell_measurement_reflns_used    2866
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      62.25
_cell_measurement_theta_min      4.888
_cell_measurement_wavelength     1.54184
_cell_volume                     4802.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0696
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0400235
_diffrn_orient_matrix_UB_12      -0.0182462
_diffrn_orient_matrix_UB_13      0.0382062
_diffrn_orient_matrix_UB_21      -0.0634642
_diffrn_orient_matrix_UB_22      0.107725
_diffrn_orient_matrix_UB_23      0.0172618
_diffrn_orient_matrix_UB_31      -0.0429199
_diffrn_orient_matrix_UB_32      -0.176651
_diffrn_orient_matrix_UB_33      0.0065712
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            16766
_diffrn_reflns_theta_full        62.46
_diffrn_reflns_theta_max         62.46
_diffrn_reflns_theta_min         4.87
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.084
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.47612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear black'
_exptl_crystal_density_diffrn    1.5
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+17.1120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.193
_refine_ls_wR_factor_ref         0.2127
_reflns_number_gt                2843
_reflns_number_total             3807
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c7dt04337f2.cif
_cod_data_source_block           1710jb10
_cod_depositor_comments
'Adding full bibliography for 7045276--7045277.cif.'
_cod_database_code               7045277