Synthesis and Structural Characterisation of the Aggregates of Benzo-1,2-Chalcogenazole 2-Oxides
Ho, Peter Cheng-Wei; Rafique, Jamal; Lee, Jiwon; Lee, Myongwon Lucia; Jenkins, Hilary A.; Britten, James F.; Braga, Antonio Luiz; Vargas-Baca, Ignacio; Dalton Trans.  (2017) –; doi:10.1039/C7DT00612H

data_7042623
_publ_section_title
;
 Synthesis and Structural Characterisation of the Aggregates of
 Benzo-1,2-Chalcogenazole 2-Oxides
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00612H
_journal_year                    2017
_chemical_formula_moiety         'C7 H5 N O Se'
_chemical_formula_sum            'C7 H5 N O Se'
_chemical_formula_weight         198.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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
_audit_creation_date             2017-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3324(9)
_cell_length_b                   8.0016(10)
_cell_length_c                   11.8324(15)
_cell_measurement_reflns_used    4214
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      3.074
_cell_volume                     694.22(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7086
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.391
_diffrn_reflns_theta_min         3.073
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.327
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1010 before and 0.0567 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1186 before and 0.0645 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 3:
 wR2(int) was 0.1040 before and 0.0575 after correction.
 The Ratio of minimum to maximum transmission is 0.58.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 25696 reflections, Rint = 0.0614
 (14788 with I > 3sig(I), Rint = 0.0507)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.622
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 665 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         7086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0447P)^2^+0.1724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.691
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                6534
_reflns_number_total             7086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00612h2.cif
_cod_data_source_block           twin4
_cod_database_code               7042623
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.415
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.399(2) 0.1669(10) 0.4343(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C3(H3)
;
_shelx_res_checksum              55405
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'