Synthetic and structural investigations of bis(N-alkyl-benzoselenadiazolium) cations.
Lee, Lucia Myongwon; Corless, Victoria; Luu, Helen; He, Allan; Jenkins, Hilary; Britten, James F.; Adam Pani, Faisal; Vargas-Baca, Ignacio; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12541–12548; doi:10.1039/c9dt02311a

data_7700707
_publ_section_title
;
 Synthetic and structural investigations of
 bis(N-alkyl-benzoselenadiazolium) cations.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12541
_journal_page_last               12548
_journal_paper_doi               10.1039/c9dt02311a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C14 H12 N4 Se2, 2.5(Cl), 4(H2 O)'
_chemical_formula_sum            'C14 H20 Cl2.5 N4 O4 Se2'
_chemical_formula_weight         554.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-04-25 deposited with the CCDC.    2019-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                77.649(5)
_cell_angle_beta                 83.560(5)
_cell_angle_gamma                71.357(4)
_cell_formula_units_Z            2
_cell_length_a                   7.624(2)
_cell_length_b                   7.942(2)
_cell_length_c                   18.270(5)
_cell_measurement_reflns_used    4346
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.008
_cell_measurement_theta_min      2.756
_cell_volume                     1022.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15656
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.285
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.969
_exptl_absorpt_correction_T_max  0.8452
_exptl_absorpt_correction_T_min  0.5094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0437 after correction.
The Ratio of minimum to maximum transmission is 0.6027.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       rod
_exptl_crystal_F_000             549
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.032
_refine_diff_density_max         2.637
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0631P)^2^+9.0032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3364
_reflns_number_total             4016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02311a2.cif
_cod_data_source_block           ll025_0m_a_1
_cod_depositor_comments
'Adding full bibliography for 7700704--7700709.cif.'
_cod_original_cell_volume        1022.9(5)
_cod_original_formula_sum        'C14 H20 Cl2.50 N4 O4 Se2'
_cod_database_code               7700707
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.452
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9722(8)
 0.0278(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3.a Free rotating group:
 O009(H00A,H00B), O00N(H00C,H00D), O00P(H00E,H00F), O00Q(H00G,H00H)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C4(H4), C13(H13), C10(H10), C12(H12), C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'