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_7243136
_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         'C36 H44 Cu6 Mo12 N20 O52 Te2, 5(H4 O2)'
_chemical_formula_sum            'C36 H64 Cu6 Mo12 N20 O62 Te2'
_chemical_formula_weight         3556.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-11-21 deposited with the CCDC.	2021-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.603(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.206(2)
_cell_length_b                   13.665(2)
_cell_length_c                   19.848(3)
_cell_measurement_reflns_used    6755
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      2.41
_cell_volume                     4233.5(10)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0231
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15668
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.530
_diffrn_reflns_theta_min         1.981
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.981
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0609 before and 0.0259 after correction.
The Ratio of minimum to maximum transmission is 0.8600.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    2.790
_exptl_crystal_description       block
_exptl_crystal_F_000             3396
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5386
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0335P)^2^+16.0367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4675
_reflns_number_total             5386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00775k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7243136--7243140.cif.'
_cod_original_cell_volume        4233.1(10)
_cod_database_code               7243136
_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,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O11 \\sim O13 \\sim O9 \\sim O2 \\sim O12 \\sim O3 \\sim O4 \\sim O7 \\sim O6
\\sim O10 \\sim O1 \\sim O8 \\sim O5 \\sim O2W \\sim O1W \\sim O3W: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H2WA(0.5) H2WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB)
4.b Free rotating group:
 O2W(H2WA,H2WB)
4.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C7(H7), C9(H9), C8(H8)
4.e X=CH2 refined with riding coordinates:
 N5(H5A,H5B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              50219
_shelx_hkl_checksum              31822
_olex2_submission_special_instructions 'No special instructions were received'