Synthesis and characterization of 4-(dimethylaminopyridyl)chalcogenides (Se, Te): X-ray structure of bis(4-dimethylamino-2-pyridyl) diselenide, bis(4-dimethylamino-2-pyridylselenenyl)methane and 4-dimethylamino-2,6-bis(methylselenenyl)pyridine
Jaspreet S. Dhau; Rupy Dhir; Amritpal Singh; Paula Brandao; Vitor Felix; Inorganica Chimica Acta 404 (2013) 160–166; doi:

data_1517761
_publ_section_title
;
 Synthesis and characterization of 4-(dimethylaminopyridyl)chalcogenides
 (Se, Te): X-ray structure of bis(4-dimethylamino-2-pyridyl) diselenide,
 bis(4-dimethylamino-2-pyridylselenenyl)methane and
 4-dimethylamino-2,6-bis(methylselenenyl)pyridine
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              160
_journal_page_last               166
_journal_volume                  404
_journal_year                    2013
_chemical_formula_sum            'C9 H14 N2 Se2'
_chemical_formula_weight         308.14
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.8530(3)
_cell_length_b                   12.4563(6)
_cell_length_c                   15.4425(8)
_cell_measurement_temperature    150(2)
_cell_volume                     1125.86(10)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'platon (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7931
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.10
_diffrn_standards_interval_count 0.5
_diffrn_standards_interval_time  20
_exptl_absorpt_coefficient_mu    6.527
_exptl_absorpt_correction_T_max  0.8805
_exptl_absorpt_correction_T_min  0.1799
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourles
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+0.0635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                2485
_reflns_number_total             2792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-404-160-166-3.cif
_cod_data_source_block           compound11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+0.0635P] 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^)+(0.0154P)^2^+0.0635P] 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      P212121
_cod_database_code               1517761