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_7712710
_publ_section_title
;
 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_absolute_configuration ad
_chemical_formula_moiety         'C70 H66 Mn4 Mo2 N22 O, 4(H2 O), 4(C2 H3 N)'
_chemical_formula_sum            'C78 H86 Mn4 Mo2 N26 O5'
_chemical_formula_weight         1879.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-18
_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                90
_cell_angle_beta                 106.344(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2700(7)
_cell_length_b                   16.3706(8)
_cell_length_c                   21.4855(11)
_cell_measurement_reflns_used    9395
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      59.51
_cell_measurement_theta_min      3.00
_cell_volume                     4478.8(4)
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            170226
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.360
_diffrn_reflns_theta_min         1.864
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19931339999999997
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.897
_exptl_absorpt_correction_T_max  0.1547
_exptl_absorpt_correction_T_min  0.0504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1561 before and 0.1011 after correction.
The Ratio of minimum to maximum transmission is 0.3258.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.098
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.107(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         20184
_refine_ls_number_restraints     764
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0558
_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^)+(0.1176P)^2^+0.1647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1766
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                15682
_reflns_number_total             20184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00610g2.cif
_cod_data_source_block           1ss_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_database_code               7712710
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.569
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.893(12)
 0.107(12)
2. 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 C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C74-C73 \\sim C74-C73A
 with sigma of 0.02
 C78A-N26A \\sim C78-N26
 with sigma of 0.02
 C78A-C77A \\sim C78-C77
 with sigma of 0.02
 N24-C73 \\sim N24A-C73A
 with sigma of 0.02
 C17-C15 \\sim C17A-C15
 with sigma of 0.02
 C37-C30 \\sim C37A-C30
 with sigma of 0.02
 N26A-C77A \\sim N26-C77
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N26A \\sim C77A \\sim C78A \\sim N26 \\sim C77 \\sim C78: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
N24 \\sim C73 \\sim C73A \\sim N24A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C20A \\sim C18 \\sim C22 \\sim C22A \\sim C20 \\sim C17A \\sim C17 \\sim C19A
\\sim C19 \\sim C21A \\sim C21 \\sim C18A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C39A \\sim C41A
\\sim C42A \\sim C40A \\sim C37A \\sim C38A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(O2) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O5) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C78A) \\sim Ueq, Uanis(N26A) \\sim Ueq, Uanis(C77A) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(N26) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C73) \\sim Ueq, Uanis(C73A) \\sim Ueq, Uanis(N24A) \\sim Ueq, Uanis(N24)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N26, C77, C78
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C73, N24, C74
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N24A, C73A, C74
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C22, C20, C19, C17, C21, C18, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C21A, C17A, C18A, C20A, C22A, C19A, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C40A, C42A, C37A, C39A, C41A, C38A, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C42, C40, C39, C37, C41, C38, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N26A, C77A, C78A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(H74D)=Sof(H74E)=Sof(H74F)=Sof(N24A)=Sof(C73A)=1-FVAR(1)
 Sof(N24)=Sof(C73)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(1)
 Sof(H15C)=Sof(C17A)=Sof(C22A)=Sof(H22C)=Sof(C21A)=Sof(H21C)=Sof(C20A)=
 Sof(H20C)=Sof(C19A)=Sof(H19C)=Sof(C18A)=Sof(H18C)=1-FVAR(2)
 Sof(H15)=Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=
 Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=FVAR(2)
 Sof(H30A)=Sof(C37A)=Sof(C42A)=Sof(H42A)=Sof(C41A)=Sof(H41A)=Sof(C40A)=
 Sof(H40A)=Sof(C39A)=Sof(H39A)=Sof(C38A)=Sof(H38A)=1-FVAR(3)
 Sof(H30)=Sof(C37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=
 Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=FVAR(3)
 Sof(N26A)=Sof(C77A)=Sof(C78A)=Sof(H78D)=Sof(H78E)=Sof(H78F)=1-FVAR(4)
 Sof(N26)=Sof(C77)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=FVAR(4)
7.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O5(H5A,H5B), O6(H6A,H6B), C74(H74A,
 H74B,H74C), C74(H74D,H74E,H74F), C78(H78A,H78B,H78C)
7.b Ternary CH refined with riding coordinates:
 C15(H15), C15(H15C), C16(H16), C29(H29), C30(H30), C30(H30A), C43(H43),
 C44(H44), C57(H57), C58(H58)
7.c Secondary CH2 refined with riding coordinates:
 N15(H15A,H15B), N16(H16A,H16B), N17(H17A,H17B), N18(H18A,H18B), N19(H19A,
 H19B), N20(H20A,H20B), N21(H21A,H21B), N22(H22A,H22B)
7.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67),
 C68(H68), C69(H69), C70(H70), C22A(H22C), C21A(H21C), C20A(H20C), C19A(H19C),
 C18A(H18C), C42A(H42A), C41A(H41A), C40A(H40A), C39A(H39A), C38A(H38A)
7.e Fitted hexagon refined as free rotating group:
 C17(C18,C19,C20,C21,C22), C37(C38,C39,C40,C41,C42), C17A(C22A,C21A,C20A,C19A,
 C18A), C37A(C42A,C41A,C40A,C39A,C38A)
7.f Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C76(H76A,H76B,H76C), C78A(H78D,H78E,H78F)
;
_shelx_res_checksum              21340
_shelx_hkl_checksum              40858
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU