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_1545713
_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         'C20 H18 B F3 N2 O2 Te2'
_chemical_formula_sum            'C20 H18 B F3 N2 O2 Te2'
_chemical_formula_weight         641.38
_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                 104.610(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2898(8)
_cell_length_b                   13.3035(13)
_cell_length_c                   11.5610(12)
_cell_measurement_reflns_used    1512
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.651
_cell_measurement_theta_min      2.888
_cell_volume                     1084.9(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7428
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.389
_diffrn_reflns_theta_min         3.000
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.733
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0618 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.8715.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 1630 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4406
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0104P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                3858
_reflns_number_total             4406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7fd00075h2.cif
_cod_data_source_block           ph540_0m_a
_cod_depositor_comments
;

2019-03-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         320.69
_cod_original_formula_moiety         '0.5(C20 H18 B F3 N2 O2 Te2)'
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C10 H9 B0.50 F1.50 N O Te'
_cod_database_code               1545713
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.611
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C4(H4A,H4B,H4C)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C6(H6), C2(H2), C10(H10), C18(H18), C7(H7), C8(H8), C9(H9),
 C20(H20), C16(H16), C19(H19), C17(H17)
;
_shelx_res_checksum              71004
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'