Crystal structure of {(<i>S</i>)-1-phenyl-<i>N</i>,<i>N</i>-bis[(pyridin-2-yl)methyl]ethanamine-κ^3^<i>N</i>,<i>N</i>',<i>N</i>''}bis(thiocyanato-κ<i>N</i>)zinc from synchrotron data
Lee, Dong Won; Shin, Jong Won; Acta Crystallographica Section E 73 (2017) 17–19; doi:10.1107/S2056989016019253

data_2241977
_publ_section_title
;
 Crystal structure of
 {(<i>S</i>)-1-phenyl-<i>N</i>,<i>N</i>-bis[(pyridin-2-yl)methyl]ethanamine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>''}bis(thiocyanato-\k<i>N</i>)zinc
 from synchrotron data
;
_journal_coeditor_code           IS5466
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              17
_journal_page_last               19
_journal_paper_doi               10.1107/S2056989016019253
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Zn (N C S)2 (C20 H21 N3)]'
_chemical_formula_moiety         'C22 H21 N5 S2 Zn'
_chemical_formula_sum            'C22 H21 N5 S2 Zn'
_chemical_formula_weight         484.93
_chemical_name_systematic
{(<i>S</i>)-1-Phenyl-<i>N</i>,<i>N</i>-bis[(pyridin-2-yl)methyl]ethanamine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>''}bis(thiocyanato-\k<i>N</i>)zinc(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.71(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.270(4)
_cell_length_b                   7.7950(16)
_cell_length_c                   14.834(3)
_cell_measurement_reflns_used    32924
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.55
_cell_measurement_theta_min      0.36
_cell_volume                     2227.2(8)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC</i>  (Shin <i>et al</i>., 2016)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11189
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         2.435
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       needle
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.346
_refine_diff_density_min         -1.029
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2026 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.010(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6035
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0509P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                5123
_reflns_number_total             6035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5466sup1.cif
_cod_data_source_block           I
_cod_database_code               2241977
_cod_database_fobs_code          2241977
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.981
_shelx_hkl_checksum              46834
_shelx_res_checksum              8637