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_7243138
_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         '2(Mo8 O26), C52 H72 Cu4 N24, 2(O)'
_chemical_formula_sum            'C52 H72 Cu4 Mo16 N24 O54'
_chemical_formula_weight         3686.53
_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             2020-12-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-12-22 deposited with the CCDC.	2021-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.734(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.790(2)
_cell_length_b                   21.231(2)
_cell_length_c                   19.024(2)
_cell_measurement_reflns_used    5256
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.27
_cell_volume                     5118.9(11)
_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 0.992
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18863
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.452
_diffrn_reflns_theta_min         1.871
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5936
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0731 before and 0.0293 after correction.
The Ratio of minimum to maximum transmission is 0.7960.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    2.392
_exptl_crystal_F_000             3544
_refine_diff_density_max         2.089
_refine_diff_density_min         -2.252
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6432
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+209.4346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4310
_reflns_number_total             6432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00775k2.cif
_cod_data_source_block           2_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7243136--7243140.cif.'
_cod_original_cell_volume        5118.9(12)
_cod_database_code               7243138
_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 C(H,H,H,H) groups, All N(H) groups,
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C0) \\sim Ueq, Uanis(C011) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00L) \\sim Ueq, Uanis(O00K) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1A) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Sof(H00H)=Sof(H00J)=Sof(O00L)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(O1A)=Sof(H00A)=1-
 FVAR(1)
 Sof(O00K)=Sof(H00V)=Sof(H00F)=Sof(H00G)=Sof(C011)=Sof(H01C)=Sof(H01D)=Sof(O1)=
 FVAR(1)
4.a Riding coordinates:
 N00V(H00V)
4.b Secondary CH2 refined with riding coordinates:
 C00X(H00B,H00C), C00Y(H00D,H00E), C00Z(H00F,H00G), C00Z(H00H,H00J), C010(H01A,
 H01B), C011(H01C,H01D), C012(H01E,H01F), C0(H0A,H0B)
4.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00L(H00L), C00R(H00R), C00S(H00S), C00U(H00U)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              441
_shelx_hkl_checksum              75236
_shelx_fab_checksum              30421
_olex2_submission_special_instructions 'No special instructions were received'