Chlorido(1-cyclopentylidene-4-ethylthiosemicarbazidato-κ^2^<i>N</i>^1^,<i>S</i>)diphenyltin(IV)
Venkatraman, Ramaiyer; Sitole, Lungile; Fronczek, Frank R.; Acta Crystallographica Section E 65 (2009) m1653–m1654; doi:10.1107/S1600536809047400

data_2224345
_publ_section_title
Chlorido(1-cyclopentylidene-4-ethylthiosemicarbazidato-\k^2^<i>N</i>^1^,<i>S</i>)diphenyltin(IV)
_journal_coeditor_code           LH2925
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1653
_journal_page_last               m1654
_journal_paper_doi               10.1107/S1600536809047400
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Sn (C6 H5)2 (C8 H14 N3 S) Cl]'
_chemical_formula_moiety         'C20 H24 Cl N3 S Sn'
_chemical_formula_sum            'C20 H24 Cl N3 S Sn'
_chemical_formula_weight         492.62
_chemical_name_systematic
;
Chlorido(1-cyclopentylidene-4-ethylthiosemicarbazidato-
\k^2^<i>N</i>^1^,<i>S</i>)diphenyltin(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 111.094(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9031(9)
_cell_length_b                   22.951(3)
_cell_length_c                   11.1381(11)
_cell_measurement_reflns_used    8037
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      34.8
_cell_measurement_theta_min      2.5
_cell_volume                     2123.4(4)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device
'Nonius KappaCCD diffractometer with an Oxford Cryosystems Cryostream cooler'
_diffrn_measurement_method       ' \w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33496
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         34.8
_diffrn_reflns_theta_min         3.0
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.64
_refine_diff_density_min         -1.38
_refine_ls_extinction_coef       0.00150(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.035
_refine_ls_R_factor_gt           0.026
_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^)+(0.0232P)^2^+1.4419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.059
_refine_ls_wR_factor_ref         0.062
_reflns_number_gt                7543
_reflns_number_total             8756
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2925.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n        '
_cod_database_code               2224345
_cod_database_fobs_code          2224345