Pentacarbonyl{tris[4-(methylsulfonyl)phenyl]stannyl}manganese(I): an unexpected tetragonal structure
Christendat, Dharamdat; Wharf, Ivor; Lebuis, Anne-Marie; Butler, Ian S.; Gilson, Denis F. R.; Acta Crystallographica Section C 58 (2002) m297–m299; doi:10.1107/S0108270102004377

data_2012695
_publ_section_title
;
 Pentacarbonyl{tris[4-(methylsulfonyl)phenyl]stannyl}manganese(I): an
 unexpected tetragonal structure
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m297
_journal_page_last               m299
_journal_paper_doi               10.1107/S0108270102004377
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Mn Sn (C7 H7 O2 S)3 (C O)5]'
_chemical_formula_moiety         'C26 H21 Mn O11 S3 Sn'
_chemical_formula_sum            'C26 H21 Mn O11 S3 Sn'
_chemical_formula_weight         779.24
_chemical_name_systematic
;
Pentacarbonyl{tris[4-(methylsulfonyl)phenyl]stannyl}manganese(I)
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.41880(10)
_cell_length_b                   22.41880(10)
_cell_length_c                   11.97640(10)
_cell_measurement_reflns_used    28577
_cell_measurement_temperature    279(2)
_cell_measurement_theta_max      73.3
_cell_measurement_theta_min      2.7
_cell_volume                     6019.37(6)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      279(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 2K/Platform'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34825
_diffrn_reflns_theta_full        73.33
_diffrn_reflns_theta_max         73.33
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        none
_diffrn_standards_number         316
_exptl_absorpt_coefficient_mu    12.467
_exptl_absorpt_correction_T_max  0.536
_exptl_absorpt_correction_T_min  0.037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.37
_refine_ls_abs_structure_details 'Flack (1983), 2802 Friedel pairs'
_refine_ls_abs_structure_Flack   0.009(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.035
_refine_ls_R_factor_gt           0.033
_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^)+(0.0544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.081
_refine_ls_wR_factor_ref         0.082
_reflns_number_gt                5643
_reflns_number_total             5976
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1638.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 'Tetragonal' changed to 'tetragonal'
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 
;
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               2012695
_cod_database_fobs_code          2012695