Main group bismuth(iii), gallium(iii) and diorganotin(iv) complexes derived from bis(2-acetylpyrazine)thiocarbonohydrazone: synthesis, crystal structures and biological evaluation.
Zhang, Nan; Tai, Yanxue; Li, Mingxue; Ma, Pengtao; Zhao, Junwei; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5182–5189; doi:10.1039/c4dt00077c

data_7029314
_publ_section_title
;
 Main group bismuth(iii), gallium(iii) and diorganotin(iv) complexes
 derived from bis(2-acetylpyrazine)thiocarbonohydrazone: synthesis,
 crystal structures and biological evaluation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5182
_journal_page_last               5189
_journal_paper_doi               10.1039/c4dt00077c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C26 H26 Ga N16 S2'
_chemical_formula_sum            'C26 H26 Ga N16 S2'
_chemical_formula_weight         696.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   13.4347(9)
_cell_length_b                   31.954(2)
_cell_length_c                   33.272(2)
_cell_measurement_reflns_used    3209
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      21.180
_cell_measurement_theta_min      2.449
_cell_volume                     14283.4(16)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            22702
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.22
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0687 before and 0.0515 after correction.
The Ratio of minimum to maximum transmission is 0.8176.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5712
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                2300
_reflns_number_total             3116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00077c.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        14283.1(16)
_cod_database_code               7029314
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C1(H1), C2(H2), C3(H3), C11(H11), C12(H12), C13(H13)
;
_smtbx_masks_special_details
;
 Highly disordered solvent was located in the structures.
 Reflection contributions from this solvent were removed
 using program OLEX2, function MSAKS, which determined
 there to be 913 electrons in 3226.7 \%A^3^ removed per unit cell. 
 One set of residual peaks did appear to one acetate ion. 
 However, this did not define the entire solvent area. 
 Thus, the total number of electrons [913] in the void per unit cell, 
 equivalent to about 913/16 = 57 per molecule unit, 
 which is attributed to one disordered acetate ion and one alcohol molecule.
 All these reported items that derive from the molecular formula 
 (e.g., F(000), density, molecular weight, etc.) are known to be incorrect.
;