Structural diversity and supramolecular architectures of Zn(ii), Cu(ii) and Ni(ii) complexes by selective control of the degree of deprotonation of diacetyl bis(4-isopropyl-3-thiosemicarbazone)
González-García, Cristina; Mendiola, M. Antonia; Perles, Josefina; López-Torres, Elena; CrystEngComm 19 (2017) 1035–; doi:10.1039/C6CE02488B

data_7227534
_publ_section_title
;
 Structural diversity and supramolecular architectures of Zn(ii), Cu(ii)
 and Ni(ii) complexes by selective control of the degree of deprotonation
 of diacetyl bis(4-isopropyl-3-thiosemicarbazone)
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1035
_journal_paper_doi               10.1039/C6CE02488B
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C14 H28 N6 Ni O S3'
_chemical_formula_weight         451.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2017-01-11 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7144(6)
_cell_length_b                   7.0324(3)
_cell_length_c                   21.4403(8)
_cell_measurement_reflns_used    3797
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      19.3697
_cell_measurement_theta_min      2.3506
_cell_volume                     2218.59(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34107
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            'brown orange'
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.729
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2467
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0484
_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^)+(0.1000P)^2^+0.8603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                1631
_reflns_number_total             2467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02488b2.cif
_cod_data_source_block           6DMSO
_cod_depositor_comments
'Adding full bibliography for 7227533--7227538.cif.'
_cod_database_code               7227534
_shelx_res_checksum              47687