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_7042622
_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         'C28 H20 N4 O4 Te4, C6 H6'
_chemical_formula_sum            'C34 H26 N4 O4 Te4'
_chemical_formula_weight         1064.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-08
_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                 95.384(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.646(3)
_cell_length_b                   17.433(2)
_cell_length_c                   10.6572(15)
_cell_measurement_reflns_used    3040
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      3.02
_cell_volume                     3448.9(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.9-0 (Bruker, 2014)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.997
_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_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13318
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.299
_diffrn_reflns_theta_min         3.206
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.393
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0463 before and 0.0317 after correction.
The Ratio of minimum to maximum transmission is 0.6097.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_description       rod
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.968
_refine_diff_density_min         -1.514
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4255
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0314P)^2^+15.4489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2913
_reflns_number_total             4255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00612h2.cif
_cod_data_source_block           ph509_0m_a
_cod_database_code               7042622
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.509
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H11(0.068) H12(0.086) H7(0.082) H6(0.092) H14(0.081) H5(0.09)
 H10(0.07) H13(0.093) H4(0.083) H3(0.067) H17(0.112) H16(0.108) H15(0.103)
 Fixed X: H11(0.5576) H12(0.5915) H7(0.2985) H6(0.1771) H14(0.7167) H5(0.1391)
 H10(0.7257) H13(0.6705) H4(0.2212) H3(0.4291) H17(0.0213) H16(0.0444)
 H15(0.0208)
 Fixed Y: H11(0.6966) H12(0.8002) H7(0.5092) H6(0.5232) H14(0.8802) H5(0.587)
 H10(0.804) H13(0.8906) H4(0.6427) H3(0.5321) H17(0.4658) H16(0.5791)
 H15(0.6935)
 Fixed Z: H11(0.2981) H12(0.1809) H7(0.1843) H6(0.2056) H14(0.4758) H5(0.3746)
 H10(0.6851) H13(0.2694) H4(0.5267) H3(0.2724) H17(0.154) H16(0.0563)
 H15(0.1509)
;
_shelx_res_checksum              90705
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'