#------------------------------------------------------------------------------
#$Date: 2023-11-07 01:57:27 +0200 (Tue, 07 Nov 2023) $
#$Revision: 287448 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/43/7714399.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7714399
loop_
_publ_author_name
'Narsimhulu, Gujju'
'Samuel, Calvin'
'Sathish, Palani'
'Dasari, Sai Hemanth Kumar'
'Krishnamoorthy, Kothandam'
'Viswanathan, Baskar'
_publ_section_title
;
 Electrocatalytic Hydrogen Evolution Mediated by an Organotelluroxane
 Macrocycle Stabilized through Secondary Interactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02746E
_journal_year                    2023
_chemical_formula_moiety         'C21 H21 O3 Te, B F4'
_chemical_formula_sum            'C21 H21 B F4 O3 Te'
_chemical_formula_weight         535.79
_chemical_name_systematic
'tris(p-methoxyphenyl)Telluronium tetraflouroborate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2022-03-21 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                110.245(2)
_cell_angle_beta                 97.9550(10)
_cell_angle_gamma                104.2830(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2455(2)
_cell_length_b                   10.5162(2)
_cell_length_c                   10.9829(2)
_cell_measurement_reflns_used    12494
_cell_measurement_temperature    106(9)
_cell_measurement_theta_max      26.8880
_cell_measurement_theta_min      2.0430
_cell_volume                     1042.82(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      106(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -46.00 -20.00   0.50    3.00    --   16.22 -67.00  57.00   52
  2  ω    -10.00  42.00   0.50    3.00    --   16.22 -67.00  57.00  104
  3  ω     50.00  75.00   0.50    3.00    --   16.22 -15.00  60.00   50
  4  ω      0.00  55.00   0.50    3.00    --  -14.97  45.00  60.00  110
  5  ω    -37.00  21.00   0.50    3.00    --  -14.97 -94.00 150.00  116
  6  ω    -63.00  -6.00   0.50    3.00    --  -14.97 -67.00  57.00  114
  7  ω    -37.00  21.00   0.50    3.00    --  -14.97 -94.00  30.00  116
  8  ω    -36.00  17.00   0.50    3.00    --   16.22 -94.00  30.00  106
  9  ω    -63.00  28.00   0.50    3.00    --   16.22 -15.00  60.00  182
 10  ω    -65.00 -18.00   0.50    3.00    --  -14.97 125.00 -30.00   94
 11  ω    -43.00 -17.00   0.50    3.00    --  -14.97 125.00 -60.00   52
 12  ω    -44.00  55.00   0.50    3.00    --  -14.97  67.00-168.00  198
 13  ω    -31.00  20.00   0.50    3.00    --  -14.97 -94.00 -90.00  102
 14  ω     32.00  58.00   0.50    3.00    --   16.22-125.00 -90.00   52
 15  ω     -6.00  44.00   0.50    3.00    --   16.22 -94.00-120.00  100
 16  ω    -41.00  59.00   0.50    3.00    --  -14.97  30.00-180.00  200
 17  ω     45.00  85.00   0.50    3.00    --   16.22  67.00-168.00   80
 18  ω     20.00  51.00   0.50    3.00    --   16.22  45.00-180.00   62
 19  ω    -56.00  32.00   0.50    3.00    --   16.22 -30.00 -90.00  176
 20  ω    -85.00  -6.00   0.50    3.00    --  -14.97 -45.00-120.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0531131000
_diffrn_orient_matrix_UB_12      -0.0176722000
_diffrn_orient_matrix_UB_13      -0.0308879000
_diffrn_orient_matrix_UB_21      0.0161002000
_diffrn_orient_matrix_UB_22      -0.0318839000
_diffrn_orient_matrix_UB_23      0.0449844000
_diffrn_orient_matrix_UB_31      -0.0485007000
_diffrn_orient_matrix_UB_32      -0.0664586000
_diffrn_orient_matrix_UB_33      -0.0454542000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15561
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.962
_diffrn_reflns_theta_min         2.039
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_recrystallization_method 'Direct evopuration'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0229P)²+1.0127P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4023
_reflns_number_total             4326
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02746e2.cif
_cod_data_source_block           vb115a
_cod_database_code               7714399
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.384
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C9(H9), C19(H19), C20(H20), C5(H5), C17(H17), C13(H13),
 C16(H16), C3(H3), C2(H2), C12(H12)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C7(H7A,H7B,H7C)
;
_olex2_exptl_crystal_mounting_method 'Mounted on glass fiber tip '
_olex2_submission_original_sample_id Gnrg-Vb194
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.947
_oxdiff_exptl_absorpt_empirical_full_min 0.658
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 0.16188(2) 0.23493(2) 0.24997(2) 0.02227(6) Uani 1 1 d . . . . .
F1 F 0.15090(17) -0.07026(17) 0.09588(17) 0.0358(4) Uani 1 1 d . . . . .
F2 F -0.0051(2) -0.28861(18) -0.03466(17) 0.0465(5) Uani 1 1 d . . . . .
F4 F 0.0775(2) -0.2358(2) 0.18252(19) 0.0550(6) Uani 1 1 d . . . . .
O3 O 0.1355(2) 0.81557(19) 0.64161(18) 0.0291(4) Uani 1 1 d . . . . .
O2 O 0.4697(2) 0.1060(2) 0.7005(2) 0.0362(5) Uani 1 1 d . . . . .
O1 O 0.6831(2) 0.3945(2) 0.0371(2) 0.0473(6) Uani 1 1 d . . . . .
F3 F -0.0680(2) -0.1277(2) 0.1202(3) 0.0752(8) Uani 1 1 d . . . . .
C8 C 0.2715(3) 0.1897(3) 0.3977(3) 0.0235(5) Uani 1 1 d . . . . .
C10 C 0.4857(3) 0.1989(3) 0.5278(3) 0.0254(6) Uani 1 1 d . . . . .
H10 H 0.581972 0.222429 0.546588 0.030 Uiso 1 1 calc R . . . .
C6 C 0.4123(3) 0.4403(3) 0.2188(3) 0.0280(6) Uani 1 1 d . . . . .
H6 H 0.386188 0.511058 0.278619 0.034 Uiso 1 1 calc R . . . .
C18 C 0.1565(3) 0.6950(3) 0.5600(3) 0.0235(6) Uani 1 1 d . . . . .
C9 C 0.4151(3) 0.2255(3) 0.4270(3) 0.0252(6) Uani 1 1 d . . . . .
H9 H 0.464492 0.267881 0.378578 0.030 Uiso 1 1 calc R . . . .
C19 C 0.2313(3) 0.6203(3) 0.6056(3) 0.0256(6) Uani 1 1 d . . . . .
H19 H 0.276113 0.655113 0.695692 0.031 Uiso 1 1 calc R . . . .
C1 C 0.3342(3) 0.2986(3) 0.1762(3) 0.0231(5) Uani 1 1 d . . . . .
C15 C 0.1716(3) 0.4409(3) 0.3817(3) 0.0225(5) Uani 1 1 d . . . . .
C20 C 0.2389(3) 0.4935(3) 0.5159(3) 0.0260(6) Uani 1 1 d . . . . .
H20 H 0.289562 0.443289 0.545969 0.031 Uiso 1 1 calc R . . . .
C5 C 0.5298(3) 0.4778(3) 0.1727(3) 0.0303(6) Uani 1 1 d . . . . .
H5 H 0.581883 0.573400 0.200968 0.036 Uiso 1 1 calc R . . . .
C17 C 0.0942(3) 0.6457(3) 0.4243(3) 0.0266(6) Uani 1 1 d . . . . .
H17 H 0.048343 0.698804 0.393360 0.032 Uiso 1 1 calc R . . . .
C11 C 0.4113(3) 0.1367(3) 0.6006(3) 0.0280(6) Uani 1 1 d . . . . .
C13 C 0.1965(3) 0.1257(3) 0.4700(3) 0.0322(6) Uani 1 1 d . . . . .
H13 H 0.100102 0.100125 0.449768 0.039 Uiso 1 1 calc R . . . .
C4 C 0.5686(3) 0.3723(3) 0.0846(3) 0.0321(7) Uani 1 1 d . . . . .
C16 C 0.1002(3) 0.5182(3) 0.3353(3) 0.0265(6) Uani 1 1 d . . . . .
H16 H 0.056833 0.484220 0.244922 0.032 Uiso 1 1 calc R . . . .
C14 C 0.6188(3) 0.1464(3) 0.7359(3) 0.0356(7) Uani 1 1 d . . . . .
H14A H 0.650468 0.100891 0.658992 0.053 Uiso 1 1 calc GR . . . .
H14B H 0.647899 0.116963 0.805895 0.053 Uiso 1 1 calc GR . . . .
H14C H 0.657458 0.248223 0.766644 0.053 Uiso 1 1 calc GR . . . .
C3 C 0.4880(3) 0.2297(3) 0.0404(3) 0.0377(7) Uani 1 1 d . . . . .
H3 H 0.513397 0.158882 -0.020063 0.045 Uiso 1 1 calc R . . . .
C2 C 0.3713(3) 0.1925(3) 0.0852(3) 0.0319(6) Uani 1 1 d . . . . .
H2 H 0.317561 0.097152 0.054857 0.038 Uiso 1 1 calc R . . . .
C12 C 0.2665(3) 0.1007(3) 0.5712(3) 0.0349(7) Uani 1 1 d . . . . .
H12 H 0.217107 0.059659 0.620433 0.042 Uiso 1 1 calc R . . . .
C21 C 0.2134(3) 0.8789(3) 0.7792(3) 0.0343(7) Uani 1 1 d . . . . .
H21A H 0.310809 0.899019 0.782859 0.051 Uiso 1 1 calc GR . . . .
H21B H 0.186221 0.813854 0.821356 0.051 Uiso 1 1 calc GR . . . .
H21C H 0.195075 0.966151 0.825019 0.051 Uiso 1 1 calc GR . . . .
C7 C 0.7757(3) 0.5355(4) 0.0855(3) 0.0481(9) Uani 1 1 d . . . . .
H7A H 0.853933 0.535087 0.046427 0.072 Uiso 1 1 calc GR . . . .
H7B H 0.807265 0.571838 0.181118 0.072 Uiso 1 1 calc GR . . . .
H7C H 0.728755 0.595149 0.061612 0.072 Uiso 1 1 calc GR . . . .
B1 B 0.0385(3) -0.1799(3) 0.0932(3) 0.0297(7) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 Te1 C15 94.95(10) . . ?
C1 Te1 C8 95.31(10) . . ?
C1 Te1 C15 97.45(10) . . ?
C18 O3 C21 117.0(2) . . ?
C11 O2 C14 117.0(2) . . ?
C4 O1 C7 118.3(3) . . ?
C9 C8 Te1 121.56(19) . . ?
C9 C8 C13 119.9(2) . . ?
C13 C8 Te1 118.5(2) . . ?
C9 C10 C11 119.4(3) . . ?
C1 C6 C5 120.3(3) . . ?
O3 C18 C19 123.7(2) . . ?
O3 C18 C17 116.1(2) . . ?
C19 C18 C17 120.1(2) . . ?
C10 C9 C8 120.6(2) . . ?
C18 C19 C20 119.5(2) . . ?
C6 C1 Te1 122.0(2) . . ?
C6 C1 C2 120.2(3) . . ?
C2 C1 Te1 117.80(19) . . ?
C20 C15 Te1 120.24(19) . . ?
C20 C15 C16 120.0(2) . . ?
C16 C15 Te1 119.50(19) . . ?
C19 C20 C15 120.4(2) . . ?
C4 C5 C6 119.6(3) . . ?
C16 C17 C18 120.3(2) . . ?
O2 C11 C10 124.2(3) . . ?
O2 C11 C12 115.8(2) . . ?
C10 C11 C12 120.0(3) . . ?
C12 C13 C8 119.5(3) . . ?
O1 C4 C5 125.2(3) . . ?
O1 C4 C3 115.1(3) . . ?
C5 C4 C3 119.7(3) . . ?
C17 C16 C15 119.6(2) . . ?
C2 C3 C4 120.7(3) . . ?
C3 C2 C1 119.4(3) . . ?
C13 C12 C11 120.5(3) . . ?
F2 B1 F1 108.6(3) . . ?
F4 B1 F1 110.7(2) . . ?
F4 B1 F2 108.2(2) . . ?
F3 B1 F1 109.2(2) . . ?
F3 B1 F2 108.9(3) . . ?
F3 B1 F4 111.2(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te1 C8 2.101(3) . ?
Te1 C1 2.100(3) . ?
Te1 C15 2.117(3) . ?
F1 B1 1.403(4) . ?
F2 B1 1.394(4) . ?
F4 B1 1.369(4) . ?
O3 C18 1.364(3) . ?
O3 C21 1.439(3) . ?
O2 C11 1.350(3) . ?
O2 C14 1.437(3) . ?
O1 C4 1.350(3) . ?
O1 C7 1.414(4) . ?
F3 B1 1.360(4) . ?
C8 C9 1.386(4) . ?
C8 C13 1.399(4) . ?
C10 C9 1.386(4) . ?
C10 C11 1.390(4) . ?
C6 C1 1.380(4) . ?
C6 C5 1.391(4) . ?
C18 C19 1.385(4) . ?
C18 C17 1.391(4) . ?
C19 C20 1.385(4) . ?
C1 C2 1.390(4) . ?
C15 C20 1.385(4) . ?
C15 C16 1.390(4) . ?
C5 C4 1.380(4) . ?
C17 C16 1.381(4) . ?
C11 C12 1.398(4) . ?
C13 C12 1.375(4) . ?
C4 C3 1.393(4) . ?
C3 C2 1.375(4) . ?
