Complexes of dimethyltin dihalides with <i>N</i>-methylpyrrolidinone, C~12~H~24~N~2~O~2~<i>X</i>~2~Sn (<i>X</i> = Cl, Br or I)
König, Uwe-Christoph; Berkei, Michael; Neikes, Frank; Preut, Hans; Mitchell, Terence Nigel; Acta Crystallographica Section C 56 (2000) 324–326; doi:10.1107/S0108270199016388

data_2010735
_publ_section_title
;
 Complexes of dimethyltin dihalides with <i>N</i>-methylpyrrolidinone,
 C~12~H~24~N~2~O~2~<i>X</i>~2~Sn (<i>X</i> = Cl, Br or I)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              324
_journal_page_last               326
_journal_paper_doi               10.1107/S0108270199016388
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[SnBr~2~(CH~3~)~2~(C~5~H~9~NO)~2~]'
_chemical_formula_sum            'C12 H24 Br2 N2 O2 Sn'
_chemical_formula_weight         506.84
_chemical_name_systematic
;
cis-dibromo-trans-dimethyl-cis-bis(N-methylpyrrolidin-2-one-O)tin(IV)
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.98(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4750(15)
_cell_length_b                   8.0300(16)
_cell_length_c                   14.977(3)
_cell_measurement_reflns_used    3025
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.54
_cell_volume                     898.4(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  'SHELXL97 and PARST95 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full .970
_diffrn_measured_fraction_theta_max .970
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
 265 frames via \w-rotation (\D\w=1\%) at different \q values
 and 2 \\times 60 s per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .005
_diffrn_reflns_av_sigmaI/netI    .043
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3025
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.870
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             492
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         .892
_refine_diff_density_min         -.850
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .370(13)
_refine_ls_extinction_coef       .0055(14)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3019
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          .040
_refine_ls_R_factor_gt           .038
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0588P)^2^+2.0195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .104
_reflns_number_gt                2893
_reflns_number_total             3019
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1448.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0588P)^2^+2.0195P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0588P)^2^+2.0195P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2010735
_cod_database_fobs_code          2010735