An Unexpected Trimethylstannylpyrrole from a Stannylated Derivative of Tosylmethyl Isocyanide (TosMIC) and Chalcone
Meetsma, A.; Dijkstra, H. P.; ten Have, R.; van Leusen, A. M.; Acta Crystallographica Section C 52 (1996) 2747–2750; doi:10.1107/S0108270196009286

data_2005591
_publ_section_title
;
 An Unexpected Trimethylstannylpyrrole from a Stannylated Derivative of
 Tosylmethyl Isocyanide (TosMIC) and Chalcone
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2747
_journal_page_last               2750
_journal_paper_doi               10.1107/S0108270196009286
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Sn (C H3)3 (C22 H20 N O3)]'
_chemical_formula_sum            'C25 H29 N O3 Sn'
_chemical_formula_weight         510.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90
_cell_angle_beta                 109.108(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4950(10)
_cell_length_b                   9.666(10)
_cell_length_c                   19.7180(10)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    130
_cell_measurement_theta_max      20.08
_cell_measurement_theta_min      17.97
_cell_volume                     2430(3)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1995)'
_computing_data_reduction        'HELENA (Spek, 1993)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'PLATON (Spek, 1994, 1996)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    DIRDIF94
_diffrn_ambient_temperature      130
_diffrn_measurement_device       'Enraf-Nonius CAD-4F'
_diffrn_measurement_method       '\w/2\q with \w width (0.85 + 0.34tan\q)\%'
_diffrn_radiation_monochromator  'perpendicular mounted graphite'
_diffrn_radiation_source         'fine focus sealed Philips Mo tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6512
_diffrn_reflns_reduction_process
;
Intensity data were corrected for Lorentz and polarization effects, scale
variation, absorption and reduced to F~o~^2^
;
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.08
_exptl_absorpt_correction_T_max  0.478
_exptl_absorpt_correction_T_min  0.225
_exptl_absorpt_correction_type   'refined (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.53
_refine_diff_density_min         -.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.071
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_hydrogen_treatment
'H atoms refined freely with individual isotropic thermal parameters'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_obs          0.0249
_refine_ls_shift/esd_max         -.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.031P)^2^+1.72P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0689
_refine_ls_wR_factor_obs         0.0586
_reflns_number_observed          4542
_reflns_number_total             5285
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1087.cif
_cod_data_source_block           CP328
_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 

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^)+(0.031P)^2^+1.72P] 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^)+(0.031P)^2^+1.72P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2430.4(2)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2005591