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_7042625
_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
'C42 H30 N6 O6 Te6, 1.78(C H2 Cl2), 0.22(H2 O1)'
_chemical_formula_sum            'C43.78 H34 Cl3.56 N6 O6.22 Te6'
_chemical_formula_weight         1635.57
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-03
_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                120
_cell_formula_units_Z            3
_cell_length_a                   14.4246(7)
_cell_length_b                   14.4246(7)
_cell_length_c                   21.3472(12)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.255
_cell_measurement_theta_min      2.510
_cell_volume                     3846.6(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0477
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            131669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.536
_diffrn_reflns_theta_min         2.510
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.605
_exptl_absorpt_correction_T_max  0.7000
_exptl_absorpt_correction_T_min  0.5727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0631 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.8181.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_description       block
_exptl_crystal_F_000             2283
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.669
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         20091
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0264P)^2^+4.2435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                17518
_reflns_number_total             20091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00612h2.cif
_cod_data_source_block           ph462_2_0m_a
_cod_original_cell_volume        3846.6(4)
_cod_database_code               7042625
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.581
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(2) 0.51(2)
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. Uiso/Uaniso restraints and constraints
Uiso(C44) = Uiso(O44A)
4. Rigid body (RIGU) restrains
 C44, Cl4, Cl3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O44A)=Sof(H44C)=Sof(H44D)=1-FVAR(1)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(Cl3)=Sof(Cl4)=FVAR(1)
6.a Free rotating group:
 O44A(H44C,H44D)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B)
6.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C4(H4), C41(H41), C12(H12), C28(H28), C32(H32), C13(H13), C5(H5),
 C6(H6), C19(H19), C14(H14), C21(H21), C40(H40), C31(H31), C20(H20), C7(H7),
 C34(H34), C3(H3), C35(H35), C17(H17), C25(H25), C11(H11), C38(H38), C33(H33),
 C26(H26), C10(H10), C27(H27), C24(H24), C39(H39)
;
_shelx_res_checksum              87338
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'