Three New MnII-[MoIII(CN)7]4– Molecular Magnets Constructed from Chiral Bidentate Chelating Ligands
Xu, Fang-Xue; Li, Ying-Lian; Wei, Xiao-Qin; Shao, Dong; Shi, Le; Wei, Haiyan; Wang, Xin-Yi; Dalton Transactions  (2023) –; doi:10.1039/D3DT00610G

data_7712711
_publ_section_title
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 Three New MnII-[MoIII(CN)7]4-- Molecular Magnets Constructed from Chiral
 Bidentate Chelating Ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00610G
_journal_year                    2023
_chemical_formula_moiety
'C19 H29.6 Mn2 Mo N11 O0.8, 2(C2 H3 N), 0.5(H2 O), 2[C2H3N], 0.5[H2O]'
_chemical_formula_sum            'C27 H43.6 Mn2 Mo N15 O1.8'
_chemical_formula_weight         812.99
_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             2023-03-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-24 deposited with the CCDC.	2023-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                71.456(2)
_cell_angle_beta                 78.641(2)
_cell_angle_gamma                88.548(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9030(6)
_cell_length_b                   14.1521(10)
_cell_length_c                   18.6565(14)
_cell_measurement_reflns_used    7089
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.35
_cell_volume                     1938.0(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS PHOTON 100'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14170
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.350
_diffrn_source                   TXS
_diffrn_source_type              'Rotaing Anode'
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1065 before and 0.0433 after correction.
The Ratio of minimum to maximum transmission is 0.6207.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.483
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7057
_refine_ls_number_restraints     641
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0585P)^2^+3.6285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1353
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5801
_reflns_number_total             7057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00610g2.cif
_cod_data_source_block           20211224xfxd3_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C27 H43.60 Mn2 Mo N15 O1.80'
_cod_database_code               7712711
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.881
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C16-C15 = C16-C17 = C18-C17 = C18-C19 = C14-C19 = C14-C15 = C15A-C14A = C19A-
 C14A = C18A-C19A = C18A-C17A = C17A-C16A = C15A-C16A
 1.53 with sigma of 0.005
 C9-C10 = C11-C10 = C11-C12 = C13-C12 = C13-C8 = C8A-C9A = C9-C8 = C8A-C13A =
 C13A-C12A = C11A-C12A = C11A-C10A = C10A-C9A
 1.53 with sigma of 0.005
 C16A-C18A
 2.6 with sigma of 0.005
 C17A-C19A
 2.6 with sigma of 0.005
 C15-C19
 2.6 with sigma of 0.005
 C16-C14
 2.6 with sigma of 0.005
 C18-C14
 2.6 with sigma of 0.005
 C13A-C11A
 2.6 with sigma of 0.005
 C10A-C12A
 2.6 with sigma of 0.005
 C11A-C9A
 2.6 with sigma of 0.005
 N8-C8 \\sim N8A-C8A
 with sigma of 0.02
 N9-C9A \\sim N9-C9
 with sigma of 0.02
 C11A-C12A \\sim C11-C12
 with sigma of 0.02
 N10-C14 \\sim N10A-C14A
 with sigma of 0.02
 C21A-C20A \\sim C21-C20
 with sigma of 0.02
 N13A-C21A \\sim N13-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N9 \\sim N8A \\sim C10 \\sim C9A \\sim C8 \\sim C13A \\sim C11A \\sim C12 \\sim
C9 \\sim C10A \\sim C11 \\sim C12A \\sim C13 \\sim C8A \\sim N8: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N11 \\sim N10A \\sim C14 \\sim C16 \\sim C15A \\sim C19A \\sim C17A \\sim C18
\\sim C15 \\sim C16A \\sim C17 \\sim C18A \\sim C19 \\sim C14A \\sim N10:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C21A \\sim C20A \\sim N13A \\sim C20 \\sim C21 \\sim N13: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C10, C11, N8, C8, C13, C12, C9, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8A, C10A, C8A, C9A, C12A, C13A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H9BC)=Sof(H9BD)=Sof(N8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9A)=Sof(C13A)=
 Sof(H13A)=Sof(H13B)=Sof(C11A)=Sof(H11E)=Sof(H11F)=Sof(C10A)=Sof(H10E)=
 Sof(H10F)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C8A)=Sof(H8A)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(C10)=Sof(H10C)=Sof(H10D)=Sof(C8)=Sof(H8)=Sof(C12)=
 Sof(H12A)=Sof(H12B)=Sof(C9)=Sof(H9)=Sof(C11)=Sof(H11G)=Sof(H11H)=Sof(C13)=
 Sof(H13C)=Sof(H13D)=Sof(N8)=Sof(H8B)=Sof(H8C)=FVAR(1)
 Sof(H11C)=Sof(H11D)=Sof(N10A)=Sof(H10A)=Sof(H10B)=Sof(C15A)=Sof(H15A)=
 Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C16A)=
 Sof(H16C)=Sof(H16D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C14A)=Sof(H14A)=1-FVAR(2)
 Sof(H11A)=Sof(H11B)=Sof(C14)=Sof(H14)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C18)=
 Sof(H18A)=Sof(H18B)=Sof(C15)=Sof(H15)=Sof(C17)=Sof(H17C)=Sof(H17D)=Sof(C19)=
 Sof(H19C)=Sof(H19D)=Sof(N10)=Sof(H10G)=Sof(H10H)=FVAR(2)
 Sof(C21A)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(N13A)=1-FVAR(3)
 Sof(C20)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21)=Sof(N13)=FVAR(3)
 Fixed Sof: O1(0.8) H1A(0.8) H1B(0.8) O2(0.5) H2A(0.5) H2B(0.5)
6.a Free rotating group:
 O2(H2A,H2B)
6.b Rotating group:
 O1(H1A,H1B)
6.c Ternary CH refined with riding coordinates:
 C14(H14), C9A(H9A), C8(H8), C15A(H15A), C9(H9), C8A(H8A), C15(H15), C14A(H14A)
6.d Secondary CH2 refined with riding coordinates:
 N9(H9BC,H9BD), N9(H9AA,H9AB), N11(H11A,H11B), N11(H11C,H11D), N8A(H8AA,H8AB),
 N10A(H10A,H10B), C10(H10C,H10D), C16(H16A,H16B), C19A(H19A,H19B), C13A(H13A,
 H13B), C17A(H17A,H17B), C18(H18A,H18B), C11A(H11E,H11F), C12(H12A,H12B),
 C10A(H10E,H10F), C11(H11G,H11H), C12A(H12C,H12D), C13(H13C,H13D), N8(H8B,H8C),
 C16A(H16C,H16D), C17(H17C,H17D), C18A(H18C,H18D), C19(H19C,H19D), N10(H10G,
 H10H)
6.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C20A(H20A,H20B,H20C), C20(H20D,H20E,H20F)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 100 electrons were 
found in a volume of 369\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[C2H3N], 0.5[H2O] 
per Asymmetric Unit which account for 98 electrons 
per unit cell.
;
_shelx_res_checksum              3346
_shelx_hkl_checksum              66754
_shelx_fab_checksum              82996
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU