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_7243137
_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         'C12 H32 Cu2 Mo6 N8 O24 Te, 6(H2 O)'
_chemical_formula_sum            'C12 H44 Cu2 Mo6 N8 O30 Te'
_chemical_formula_weight         1610.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-11-23 deposited with the CCDC.	2021-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.1000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4645(7)
_cell_length_b                   14.6884(10)
_cell_length_c                   13.0321(9)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.39
_cell_volume                     1995.2(2)
_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 0.998
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13863
_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         28.278
_diffrn_reflns_theta_min         2.094
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.691
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4686
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0941 before and 0.0336 after correction.
The Ratio of minimum to maximum transmission is 0.6284.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    2.681
_exptl_crystal_description       block
_exptl_crystal_F_000             1548
_refine_diff_density_max         0.807
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4930
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0241P)^2^+3.6327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4585
_reflns_number_total             4930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00775k2.cif
_cod_data_source_block           2_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7243136--7243140.cif.'
_cod_database_code               7243137
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O00L) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Free rotating group:
 O00L(H00A,H00B), O00M(H00C,H00D), O00O(H00E,H00F)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C2(H2A,H2B), C6(H6A,H6B), C4(H4C,H4D), C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1)
3.d X=CH2 refined with riding coordinates:
 N4(H4A,H4B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92115
_shelx_hkl_checksum              9203
_olex2_submission_special_instructions 'No special instructions were received'