Mono- and Hexanuclear Zinc Halide Complexes with Soft Thiopyridazine Based Scorpionate Ligands
Tuchler, M.; Rambock, M.; Glanzer, S.; Zangger, K.; Belaj, F.; Mosch-Zanetti, N.C.; Inorganics 7 (2019) 24–; doi:10.3390/inorganics7020024

data_1556663
_publ_section_title
;
 Mono- and Hexanuclear Zinc Halide Complexes with Soft Thiopyridazine
 Based Scorpionate Ligands
;
_journal_name_full               Inorganics
_journal_page_first              24
_journal_paper_doi               10.3390/inorganics7020024
_journal_volume                  7
_journal_year                    2019
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C36 H54 B Br N8 S4 Zn'
_chemical_formula_sum            'C36 H54 B Br N8 S4 Zn'
_chemical_formula_weight         883.20
_chemical_name_common
; bromo-(6-tert-butyl-4-methyl-3(2H)-pyridazine-thionato-S)-[hydri-
do-tris(6-tert-butyl-4-methyl-3(2H)-pyridazine-thionato-H,S,S')-borate]-zinc
;
_chemical_name_systematic
; bromo-(6-tert-butyl-4-methyl-3(2H)-pyridazine-thionato-S)-[hydri-
do-tris(6-tert-butyl-4-methyl-3(2H)-pyridazine-thionato-H,S,S')-borate]-zinc
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6456(19)
_cell_length_b                   16.9851(19)
_cell_length_c                   34.357(4)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.32
_cell_measurement_theta_min      2.40
_cell_volume                     9713.7(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0946
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            65878
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       needle
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.078(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         16976
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0626P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                11043
_reflns_number_total             16976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-24.cif
_cod_data_source_block           MR55B
_cod_original_cell_volume        9713.6(19)
_cod_database_code               1556663
_shelx_estimated_absorpt_t_min   0.760
_shelx_estimated_absorpt_t_max   0.814
_shelxl_version_number           2014/6
_shelx_res_checksum              44065
_shelx_hkl_checksum              34842