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_1545711
_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 B2 F6 N2 O3 Te2, 2(C27 H37 N2), 2(C7 H8)'
_chemical_formula_sum            'C88 H108 B2 F6 N6 O3 Te2'
_chemical_formula_weight         1688.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 107.7730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2007(6)
_cell_length_b                   20.9116(10)
_cell_length_c                   17.3413(8)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.285
_cell_measurement_theta_min      2.305
_cell_volume                     4213.2(3)
_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 0.997
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57637
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.387
_diffrn_reflns_theta_min         2.620
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0608 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.9081. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 7535 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         17086
_refine_ls_number_restraints     833
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.1624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.982
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                16188
_reflns_number_total             17086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7fd00075h2.cif
_cod_data_source_block           ph574_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         844.31
_cod_original_formula_moiety
'0.5(C20 H18 B2 F6 N2 O3 Te2), C27 H37 N2, C7 H8'
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C44 H54 B F3 N3 O1.50 Te'
_cod_database_code               1545711
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.805
_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 Ternary CH refined with riding coordinates:
 C57(H57), C42(H42), C69(H69), C72(H72), C60(H60), C30(H30), C33(H33), C45(H45)
3.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C48(H48), C12(H12), C2(H2), C23(H23), C26(H26), C20(H20), C54(H54),
 C27(H27), C19(H19), C66(H66), C67(H67), C53(H53), C38(H38), C17(H17), C22(H22),
  C18(H18), C55(H55), C39(H39), C65(H65), C16(H16), C9(H9), C10(H10), C40(H40),
 C49(H49), C28(H28), C88(H88), C81(H81), C50(H50), C8(H8), C87(H87), C6(H6),
 C84(H84), C85(H85), C7(H7), C79(H79), C80(H80), C86(H86), C78(H78), C77(H77)
3.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C14(H14A,H14B,H14C), C31(H31A,H31B,H31C), C70(H70A,H70B,
 H70C), C4(H4A,H4B,H4C), C71(H71A,H71B,H71C), C43(H43A,H43B,H43C), C74(H74A,
 H74B,H74C), C73(H73A,H73B,H73C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C),
 C61(H61A,H61B,H61C), C59(H59A,H59B,H59C), C46(H46A,H46B,H46C), C44(H44A,H44B,
 H44C), C47(H47A,H47B,H47C), C82(H82A,H82B,H82C), C62(H62A,H62B,H62C), C75(H75A,
 H75B,H75C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              91406
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'