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_1517759
_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            'C14 H18 N4 Se2'
_chemical_formula_weight         400.24
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.933(8)
_cell_angle_beta                 79.358(8)
_cell_angle_gamma                85.138(8)
_cell_formula_units_Z            2
_cell_length_a                   8.5245(17)
_cell_length_b                   8.5360(16)
_cell_length_c                   10.7494(19)
_cell_measurement_temperature    150(2)
_cell_volume                     762.7(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Platon (Speck, 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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10404
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.94
_diffrn_standards_interval_count 0.5
_diffrn_standards_interval_time  30
_exptl_absorpt_coefficient_mu    4.843
_exptl_absorpt_correction_T_max  0.8299
_exptl_absorpt_correction_T_min  0.4760
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.728
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+3.4473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                2334
_reflns_number_total             2669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-404-160-166-1.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+3.4473P] 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^)+(0.0714P)^2^+3.4473P] 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-1
_cod_database_code               1517759