α-Organoelement Nitrones: Synthesis, Properties, and IR and13C NMR Spectral and X-ray Structural Characterization†
Voinov, Maxim A.; Shevelev, Tikhon G.; Rybalova, Tatyana V.; Gatilov, Yury V.; Pervukhina, Natalie V.; Burdukov, Aleksei B.; Grigor'ev, Igor A.; Organometallics 26 (2007) 1607–; doi:10.1021/om060883o

data_4072623
_publ_section_title
;
 \a-Organoelement Nitrones:&#x00A0; Synthesis, Properties, and IR and13C
 NMR Spectral and X-ray Structural Characterization&#x2020;
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1607
_journal_paper_doi               10.1021/om060883o
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C16 H28 Hg N2 O2'
_chemical_formula_sum            'C16 H28 Hg N2 O2'
_chemical_formula_weight         480.99
_chemical_melting_point          482
_chemical_name_systematic
; 
 Bis-(2,2,4,4-tetramethyl-3,4-dihydro-2H-pyrrole-1-oxide-5-yl)-mercurio 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.862(4)
_cell_length_b                   11.552(3)
_cell_length_c                   13.875(5)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      13.1
_cell_volume                     1858.4(11)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4665
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        4.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.288
_exptl_absorpt_correction_T_max  0.2218
_exptl_absorpt_correction_T_min  0.0627
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            grey-yellow
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'unregular prism'
_exptl_crystal_F_000             936
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.797
_refine_diff_density_min         -1.598
_refine_diff_density_rms         0.239
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_coef       0.0000(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4447
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+14.1811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                4116
_reflns_number_total             4447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060883osi20060926_012501.cif
_cod_data_source_block           compound_9k_Voinov
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z 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_cell_volume        1858.3(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4072623