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_7243139
_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         'Mo4 O13, C13 H16 Cu N4 O2'
_chemical_formula_sum            'C13 H16 Cu Mo4 N4 O15'
_chemical_formula_weight         915.60
_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             2020-12-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-12-02 deposited with the CCDC.	2021-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.6850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7719(6)
_cell_length_b                   18.3338(10)
_cell_length_c                   12.7561(7)
_cell_measurement_reflns_used    2309
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.69
_cell_measurement_theta_min      2.34
_cell_volume                     2307.0(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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0561
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16932
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.338
_diffrn_reflns_theta_min         2.067
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.105
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6720
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0533 before and 0.0339 after correction.
The Ratio of minimum to maximum transmission is 0.9012.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    2.636
_exptl_crystal_F_000             1756
_refine_diff_density_max         0.694
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5751
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0275P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3920
_reflns_number_total             5751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00775k2.cif
_cod_data_source_block           2_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7243136--7243140.cif.'
_cod_database_code               7243139
_shelx_shelxl_version_number     2018/3
_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, All O(H,H) groups
2. Restrained distances
 Cu05-H00A \\sim Cu05-H00B
 with sigma of 0.02
3.a Free rotating group:
 O00C(H00A,H00B)
3.b Rotating group:
 O00H(H00C,H00D)
3.c Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00Q(H00Q), C00S(H00S), C00T(H00T), C00U(H00U), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C010(H010)
3.d Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C)
;
_shelx_res_checksum              21710
_shelx_hkl_checksum              85321
_olex2_submission_special_instructions 'No special instructions were received'