FDHALO17: Building new discrete supramolecular assemblies through the interaction of iso-tellurazole N-oxides with Lewis acids and bases
Ho, Peter Cheng-Wei; Jenkins, Hilary A.; Britten, James F.; Vargas-Baca, Ignacio; Faraday Discuss.  (2017) –; doi:10.1039/C7FD00075H

data_1545712
_publ_section_title
;
 FDHALO17: Building new discrete supramolecular assemblies through the
 interaction of iso-tellurazole N-oxides with Lewis acids and bases
;
_journal_name_full               'Faraday Discuss.'
_journal_paper_doi               10.1039/C7FD00075H
_journal_year                    2017
_chemical_formula_moiety         'C17 H19 B F3 N3 O Te, C H Cl3'
_chemical_formula_sum            'C18 H20 B Cl3 F3 N3 O Te'
_chemical_formula_weight         596.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-15 deposited with the CCDC.
2017-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2886(2)
_cell_length_b                   15.0565(3)
_cell_length_c                   14.7817(3)
_cell_measurement_reflns_used    9011
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.736
_cell_measurement_theta_min      2.705
_cell_volume                     2289.37(8)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            85052
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.998
_diffrn_reflns_theta_min         1.980
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.689
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0593 before and 0.0489 after correction.
The Ratio of minimum to maximum transmission is 0.9184.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_refine_diff_density_max         1.583
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 6567 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         14583
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0299P)^2^+1.7543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14102
_reflns_number_total             14583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7fd00075h2.cif
_cod_data_source_block           ph538_0m_b
_cod_database_code               1545712
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C18(H18), C36(H36)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C30(H30), C32(H32), C28(H28), C2(H2), C8(H8), C9(H9), C10(H10),
 C25(H25), C20(H20), C27(H27), C33(H33), C14(H14), C24(H24), C26(H26), C11(H11),
  C7(H7), C29(H29), C6(H6), C15(H15)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C4(H4A,H4B,H4C), C34(H34A,H34B,
 H34C), C22(H22A,H22B,H22C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              75158
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'