High Z’ structures of 1,2,3,5-dithiadiazolyls and of 1,2,3,5-diselenadiazolyls containing the first structurally characterized monomeric diselenadiazolyls
Boeré, René; Hill, Nathan D. D.; CrystEngComm  (2017) –; doi:10.1039/C7CE00863E

data_7228524
_publ_section_title
;
 High Z&#x2019; structures of 1,2,3,5-dithiadiazolyls and of
 1,2,3,5-diselenadiazolyls containing the first structurally characterized
 monomeric diselenadiazolyls
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00863E
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         Se
_chemical_formula_sum            Se
_chemical_formula_weight         78.96
_chemical_melting_point          494
_chemical_name_common            'Grey selenium'
_chemical_name_systematic        Selenium
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-06-19 deposited with the CCDC.
2017-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   4.3125(3)
_cell_length_b                   4.3125(3)
_cell_length_c                   4.9711(4)
_cell_measurement_reflns_used    757
_cell_measurement_temperature    99.99(14)
_cell_measurement_theta_max      75.6520
_cell_measurement_theta_min      11.8060
_cell_volume                     80.065(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -1.00  74.00   0.50    0.50    --    4.52  19.00  90.00  150
  2  \w      1.00  71.00   0.50    0.50    --    4.52  38.00-180.00  140
  3  \w     36.00 175.00   0.50    0.91    --  105.46   0.00  90.00  278
  4  \w     97.00 174.00   0.50    0.91    --  105.46  15.00-180.00  154
  5  \w     41.00 110.00   0.50    0.91    --  105.46 -45.00 -90.00  138
  6  \w      1.00  71.00   0.50    0.50    --    4.52  38.00-120.00  140
  7  \w     -1.00  74.00   0.50    0.50    --    4.52  19.00   0.00  150
  8  \w     37.00 109.00   0.50    0.91    --  105.46 -94.00-180.00  144
  9  \w     43.00 119.00   0.50    0.91    --  105.46 -61.00   0.00  152
 10  \w     37.00 109.00   0.50    0.91    --  105.46 -30.00-150.00  144
 11  \w     92.00 168.00   0.50    0.91    --  105.46  61.00 -90.00  152
 12  \w    -45.00  14.00   0.50    0.50    --   -4.52 106.00  40.00  118
 13  \w    -28.00  28.00   0.50    0.50    --    4.52  92.00 144.00  112
 14  \w     97.00 174.00   0.50    0.91    --  105.46  15.00-120.00  154
 15  \w     40.00 122.00   0.50    0.91    --  105.46-125.00  90.00  164
 16  \w    101.00 170.00   0.50    0.91    --  105.46  45.00 120.00  138
 17  \w    102.00 174.00   0.50    0.91    --  105.46  30.00 -60.00  144
 18  \w    -68.00   7.00   0.50    0.50    --   -4.52 -57.00-150.00  150
 19  \w      1.00  71.00   0.50    0.50    --    4.52  36.00  19.00  140
 20  \w     92.00 168.00   0.50    0.91    --  105.46  61.00 -30.00  152
 21  \w     82.00 170.00   0.50    0.91    --  105.46  77.00-150.00  176
 22  \w     97.00 174.00   0.50    0.91    --  105.46  15.00  30.00  154
 23  \w     43.00 119.00   0.50    0.91    --  105.46 -61.00-180.00  152
 24  \w    -25.00  29.00   0.50    0.50    --    4.52 -79.00 -79.00  108
 25  \w    -62.00   8.00   0.50    0.50    --    4.52 -38.00 -60.00  140
 26  \w     82.00 170.00   0.50    0.91    --  105.46  77.00 150.00  176
 27  \w    102.00 174.00   0.50    0.91    --  105.46  30.00  90.00  144
 28  \w     92.00 168.00   0.50    0.91    --  105.46  61.00-120.00  152
 29  \w     40.00 122.00   0.50    0.91    --  105.46-125.00-150.00  164
 30  \w    -64.00  10.00   0.50    0.50    --    4.52 -19.00 120.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at zero, Pilatus 200/300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0956512000
_diffrn_orient_matrix_UB_12      0.3951188000
_diffrn_orient_matrix_UB_13      -0.0125151000
_diffrn_orient_matrix_UB_21      -0.1614171000
_diffrn_orient_matrix_UB_22      -0.0611764000
_diffrn_orient_matrix_UB_23      -0.2847260000
_diffrn_orient_matrix_UB_31      -0.3670447000
_diffrn_orient_matrix_UB_32      -0.1018102000
_diffrn_orient_matrix_UB_33      0.1220775000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0911
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1066
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.668
_diffrn_reflns_theta_min         11.913
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    39.344
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    4.913
_exptl_crystal_description       Needle
_exptl_crystal_F_000             102
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.423
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.365
_refine_ls_extinction_coef       0.018(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.381
_refine_ls_matrix_type           full
_refine_ls_number_parameters     7
_refine_ls_number_reflns         120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.381
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0711P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.481
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                120
_reflns_number_total             120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00863e2.cif
_cod_data_source_block           Se
_cod_original_cell_volume        80.064(11)
_cod_database_code               7228524
_chemical_oxdiff_formula         Se
_chemical_oxdiff_usercomment
'Clumps of black needles from "3x sublimed 5tBu Se diradical" sealed tube'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;
_shelx_res_checksum              62866
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.982
_oxdiff_exptl_absorpt_empirical_full_min 0.611