Crystal structure of [butane-2,3-dione bis(4-methylthiosemicarbazonato)-κ^4^<i>S</i>,<i>N</i>^1^,<i>N</i>^1'^,<i>S</i>'](pyridine-κ<i>N</i>)zinc(II)
Brown, Oliver C.; Tocher, Derek A.; Blower, Philip J.; Went, Michael J.; Acta Crystallographica Section E 71 (2015) 1349–1351; doi:10.1107/S2056989015019234

data_2241225
_publ_section_title
;
 Crystal structure of [butane-2,3-dione
 bis(4-methylthiosemicarbazonato)-\k^4^<i>S</i>,<i>N</i>^1^,<i>N</i>^1'^,<i>S</i>'](pyridine-\k<i>N</i>)zinc(II)
;
_journal_coeditor_code           PJ2023
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1349
_journal_page_last               1351
_journal_paper_doi               10.1107/S2056989015019234
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Zn (C8 H14 N6 S2) (C5 H5 N1)]'
_chemical_formula_moiety         'C13 H19 N7 S2 Zn'
_chemical_formula_sum            'C13 H19 N7 S2 Zn'
_chemical_formula_weight         402.84
_chemical_name_systematic
'[Butane-2,3-dione bis(4-methylthiosemicarbazonato)-\k^4^<i>S</i>,<i>N</i>^1^,<i>N</i>^1'^,<i>S</i>'](pyridine-\k<i>N</i>)zinc(II)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.756(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1466(2)
_cell_length_b                   13.9076(3)
_cell_length_c                   12.7775(3)
_cell_measurement_reflns_used    6492
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      73.0170
_cell_measurement_theta_min      4.7770
_cell_volume                     1743.63(7)
_computing_cell_refinement
;
(CrysAlis PRO; Agilent, 2014)
;
_computing_data_collection
;
(CrysAlis PRO; Agilent, 2014)
;
_computing_data_reduction
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(CrysAlis PRO; Agilent, 2014)
;
_computing_molecular_graphics
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<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
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<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
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;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 5.2031
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova Dual Source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12050
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.605
_diffrn_reflns_theta_min         4.787
_exptl_absorpt_coefficient_mu    4.272
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       needle
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.417
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0320P)^2^+1.1359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                3020
_reflns_number_total             3445
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pj2023sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1743.64(7)
_cod_database_code               2241225
_shelx_hkl_checksum              95118
_shelx_res_checksum              33406
_shelxl_version_number           .2013
_cod_database_fobs_code 2241225