Five compounds based on [TeMo6O24]6− and [β-Mo8O26]4− anions synthesized by using different symmetrical and asymmetric N-donor ligands
Ying, Jun; Sun, Chenxi; Jin, Liang; Tian, Aixiang; Wang, Xiuli; CrystEngComm 23 (2021) 5385–5396; doi:10.1039/D1CE00775K

data_7243140
_publ_section_title
;
 Five compounds based on [TeMo6O24]6&#x2212; and [\b-Mo8O26]4&#x2212;
 anions synthesized by using different symmetrical and asymmetric N-donor
 ligands
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              5385
_journal_page_last               5396
_journal_paper_doi               10.1039/D1CE00775K
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety
'C26 H38 Cu4 Mo6 N12 O30 Te, Cu H4 Mo6 O26 Te'
_chemical_formula_sum            'C26 H42 Cu5 Mo12 N12 O56 Te2'
_chemical_formula_weight         3142.89
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-12 deposited with the CCDC.	2021-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                77.836(2)
_cell_angle_beta                 72.274(2)
_cell_angle_gamma                85.532(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1044(14)
_cell_length_b                   11.8366(15)
_cell_length_c                   13.6033(17)
_cell_measurement_reflns_used    4308
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.52
_cell_volume                     1664.7(4)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11917
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.361
_diffrn_reflns_theta_min         1.760
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.722
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0850 before and 0.0297 after correction.
The Ratio of minimum to maximum transmission is 0.7786.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.135
_exptl_crystal_description       block
_exptl_crystal_F_000             1483
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.940
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         8236
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      7.090
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0394P)^2^+2.5545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6236
_reflns_number_total             8236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00775k2.cif
_cod_data_source_block           2_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7243136--7243140.cif.'
_cod_database_code               7243140
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-O1_$1
 2.8 with sigma of 0.01
 Cu2-H2Wa \\sim Cu2-H2Wb
 with sigma of 0.02
3.a Free rotating group:
 O2W(H2Wa,H2Wb)
3.b Rotating group:
 O1W(H1Wa,H1Wb), O3W(H3Wa,H3Wb)
3.c Ternary CH refined with riding coordinates:
 N1(H1)
3.d Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b)
3.e Aromatic/amide H refined with riding coordinates:
 C12(H12), C2(H2), C3(H3), C7(H7), C5(H5), C1(H1a), C13(H13), C11(H11)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94498
_shelx_hkl_checksum              37059
_olex2_submission_special_instructions 'No special instructions were received'