Polymeric polyiodo-chlorotellurates(iv): new supramolecular hybrids in halometalate chemistry
Korobeynikov, Nikita A.; Usoltsev, Andrey N.; Sokolov, Maxim N.; Novikov, Alexander S.; Adonin, Sergey A.; CrystEngComm 26 (2024) 2018–2024; doi:10.1039/D4CE00088A

data_7248277
_publ_section_title
;
 Polymeric polyiodo-chlorotellurates(iv): new supramolecular hybrids in
 halometalate chemistry
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2018
_journal_page_last               2024
_journal_paper_doi               10.1039/D4CE00088A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'I2, Cl6 Te, 2(C3 H10 N)'
_chemical_formula_sum            'C6 H20 Cl6 I2 N2 Te'
_chemical_formula_weight         714.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-24 deposited with the CCDC.	2024-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.5880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6722(2)
_cell_length_b                   9.9937(2)
_cell_length_c                   17.2207(3)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      33.15
_cell_measurement_theta_min      2.37
_cell_volume                     2128.44(7)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30325
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.153
_diffrn_reflns_theta_min         1.647
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.038
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0895 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.8820.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.834
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         8123
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+1.5788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6710
_reflns_number_total             8123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00088a2.cif
_cod_data_source_block           nk1016
_cod_depositor_comments
'Adding full bibliography for 7248275--7248279.cif.'
_cod_database_code               7248277
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C4 \\sim N2A-C4A
 with sigma of 0.02
 N2-C5 \\sim N2A-C5A
 with sigma of 0.02
 N2-C6 \\sim N2A-C6A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.04
 C4-C6 \\sim C4A-C6A
 with sigma of 0.04
 C5-C6 \\sim C5A-C6A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(N2B) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N2(0.333333) H2(0.333333) C4(0.333333) H4A(0.333333) H4B(0.333333)
 H4C(0.333333) C5(0.333333) H5A(0.333333) H5B(0.333333) H5C(0.333333)
 C6(0.333333) H6A(0.333333) H6B(0.333333) H6C(0.333333) N2A(0.333333)
 H3(0.333333) C4A(0.333333) H4D(0.333333) H4E(0.333333) H4F(0.333333)
 C5A(0.333333) H5D(0.333333) H5E(0.333333) H5F(0.333333) C6A(0.333333)
 H6D(0.333333) H6E(0.333333) H6F(0.333333) N2B(0.333333) H4(0.333333)
 C5B(0.333333) H5G(0.333333) H5H(0.333333) H5I(0.333333) C6B(0.333333)
 H6G(0.333333) H6H(0.333333) H6I(0.333333) C4B(0.333333) H4G(0.333333)
 H4H(0.333333) H4I(0.333333)
6.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N2A(H3), N2B(H4)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3C,H3B,H3A), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C4A(H4D,H4E,H4F), C5A(H5D,H5E,H5F), C6A(H6D,H6E,
 H6F), C5B(H5G,H5H,H5I), C6B(H6G,H6H,H6I), C4B(H4G,H4H,H4I)
;
_shelx_res_checksum              83447
_olex2_submission_special_instructions 'No special instructions were received'