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_7042624
_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'
_chemical_formula_sum            'C28 H20 N4 O4 Te4'
_chemical_formula_weight         986.88
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-21
_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                106.411(2)
_cell_angle_beta                 102.489(2)
_cell_angle_gamma                90.001(2)
_cell_formula_units_Z            1
_cell_length_a                   7.2250(2)
_cell_length_b                   8.7915(3)
_cell_length_c                   12.1257(4)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      2.56
_cell_volume                     719.81(4)
_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      100.15
_diffrn_measured_fraction_theta_full 0.998
_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  0.0239
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23510
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.131
_diffrn_reflns_theta_min         2.894
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.054
_exptl_absorpt_correction_T_max  0.8668
_exptl_absorpt_correction_T_min  0.5443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0387 before and 0.0347 after correction.
The Ratio of minimum to maximum transmission is 0.6279.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5456
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4690
_reflns_number_total             5456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00612h2.cif
_cod_data_source_block           ph462yellow_b
_cod_database_code               7042624
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.418
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10(0.027) H5(0.05) H11(0.03) H7(0.042) H12(0.034) H6(0.052)
 H4(0.038) H14(0.031) H13(0.033) H3(0.034)
 Fixed X: H10(0.0906) H5(1.3298) H11(0.4353) H7(0.949) H12(0.4628) H6(1.2286)
 H4(1.1502) H14(0.2088) H13(0.3576) H3(0.6587)
 Fixed Y: H10(0.0652) H5(0.9083) H11(0.1466) H7(0.7442) H12(-0.1266)
 H6(0.8904) H4(0.7813) H14(-0.1816) H13(-0.291) H3(0.5686)
 Fixed Z: H10(0.3377) H5(1.0058) H11(0.7877) H7(1.1519) H12(0.7426) H6(1.1719)
 H4(0.8154) H14(0.4003) H13(0.5486) H3(1.0165)
;
_shelx_res_checksum              54324
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'