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_7712712
_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, 4.5(H2 O), 4(C2 H3 N)'
_chemical_formula_sum            'C78 H87 Mn4 Mo2 N26 O5.5'
_chemical_formula_weight         1888.37
_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                 105.389(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2786(12)
_cell_length_b                   16.2861(13)
_cell_length_c                   21.4317(19)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      58.20
_cell_measurement_theta_min      3.01
_cell_volume                     4468.6(7)
_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 0.990
_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  0.0827
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            139140
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.538
_diffrn_reflns_theta_min         1.860
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.912
_exptl_absorpt_correction_T_max  0.3104
_exptl_absorpt_correction_T_min  0.1719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1589 before and 0.1072 after correction.
The Ratio of minimum to maximum transmission is 0.5538.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1930
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.124
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.134(14)
_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     1299
_refine_ls_number_reflns         19979
_refine_ls_number_restraints     2210
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+0.8899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.2036
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                13775
_reflns_number_total             19979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00610g2.cif
_cod_data_source_block           1rr_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        'C78 H87 Mn4 Mo2 N26 O5.50'
_cod_database_code               7712712
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.639
_shelx_estimated_absorpt_t_min   0.568
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.866(14)
 0.134(14)
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 O(H,H) groups
3. Shared sites
{C78, C78A}
4. Restrained distances
 N10A-Mo2A
 3.4 with sigma of 0.01
 N26-C77 \\sim N26A-C77A
 with sigma of 0.02
 C78-C77 \\sim C78A-C77A
 with sigma of 0.02
 Mo2-N14B \\sim N14A-Mo2A
 with sigma of 0.02
 Mo2-Mo2A \\sim Mo2A-N10A
 with sigma of 0.02
 N26-C78 \\sim N26A-C78A
 with sigma of 0.02
 Mo2-C9B \\sim Mo2A-C9A \\sim Mo2A-C8A \\sim Mo2-C8B \\sim Mo2A-C4A \\sim
Mo2-C4B \\sim Mo2A-C10A ~
 Mo2-C10B \\sim Mo2-C3B \\sim Mo2A-C3A \\sim Mo2-C14B \\sim Mo2A-C14A \\sim
Mo2A-C11A \\sim Mo2-C11B
 with sigma of 0.02
 N9A-Mo2A \\sim N9B-Mo2 \\sim Mo2-N3B \\sim Mo2A-N3A \\sim N8A-Mo2A \\sim
N8B-Mo2 \\sim N11B-Mo2 ~
 N11A-Mo2A \\sim Mo2-N4B \\sim Mo2A-N4A
 with sigma of 0.02
 N9B-C9B \\sim N9A-C9A \\sim N8B-C8B \\sim N8A-C8A \\sim N4B-C4B \\sim N4A-C4A
\\sim N10A-C10A \\sim N10B-
 C10B \\sim N3B-C3B \\sim N3A-C3A \\sim N14B-C14B \\sim N14A-C14A \\sim
N11B-C11B \\sim N11A-C11A
 with sigma of 0.02
 C59A-C57 \\sim C59-C57
 with sigma of 0.02
 C62A-C61A \\sim C74-C73 \\sim C74A-C73A
 with sigma of 0.02
 N24-C74 \\sim N24A-C74A
 with sigma of 0.02
 N24-C73 \\sim N24A-C73A
 with sigma of 0.02
 Mn2-H1A \\sim Mn2-H1B
 with sigma of 0.02
5. 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
N3B \\sim C3B \\sim C3A \\sim N3A \\sim N10B \\sim C10B \\sim C10A \\sim N10A
\\sim N4B \\sim C4B \\sim C4A \\sim N4A \\sim N8B \\sim C8B \\sim C8A \\sim N8A
\\sim N9B \\sim C9B \\sim C9A \\sim N9A \\sim N14B \\sim C14B \\sim C14A \\sim
N14A \\sim N11B \\sim C11B \\sim C11A \\sim N11A: 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 C38A \\sim C39A
\\sim C40A \\sim C41A \\sim C42A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C59A \\sim C60A
\\sim C61A \\sim C62A \\sim C63A \\sim C64A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N25A \\sim C75A \\sim C76A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C73A \\sim N24A \\sim C74A \\sim C73 \\sim N24 \\sim C74: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(N26A) \\sim Ueq, Uanis(C77A) \\sim Ueq, Uanis(C78A) \\sim Ueq, Uanis(N26)
\\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N25A) \\sim Ueq, Uanis(C75A) \\sim Ueq, Uanis(C76A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C78) = Uanis(C78A)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N26, C77, C78
 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
 C39A, C42A, C40A, C38A, C41A, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C37, C41, C40, C38, C42, C39, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C64, C62, C61, C59, C63, C60, C57
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C64A, C62A, C61A, C59A, C63A, C60A, C57
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N25A, C75A, C76A
 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
 C73A, N24A, C74A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
7. Others
 Sof(Mo2A)=Sof(C3A)=Sof(N3A)=Sof(C10A)=Sof(N10A)=Sof(C4A)=Sof(N4A)=Sof(C14A)=
 Sof(N14A)=Sof(C8A)=Sof(N8A)=Sof(C9A)=Sof(N9A)=Sof(C11A)=Sof(N11A)=1-FVAR(1)
 Sof(Mo2)=Sof(N9B)=Sof(N14B)=Sof(N11B)=Sof(N8B)=Sof(N4B)=Sof(N10B)=Sof(N3B)=
 Sof(C9B)=Sof(C14B)=Sof(C11B)=Sof(C8B)=Sof(C4B)=Sof(C10B)=Sof(C3B)=FVAR(1)
 Sof(N26A)=Sof(C77A)=Sof(C78A)=Sof(H78D)=Sof(H78E)=Sof(H78F)=1-FVAR(2)
 Sof(N26)=Sof(C77)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=FVAR(2)
 Sof(H30A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=
 Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)=1-FVAR(3)
 Sof(H30)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=
 Sof(H41)=Sof(C42)=Sof(H42)=FVAR(3)
 Sof(H57A)=Sof(C59A)=Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(H61A)=Sof(C62A)=
 Sof(H62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=Sof(H64A)=1-FVAR(4)
 Sof(H57)=Sof(C59)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=
 Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=FVAR(4)
 Sof(C73A)=Sof(N24A)=Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(5)
 Sof(N24)=Sof(C73)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(5)
 Fixed Sof: O4(0.5) H4A(0.5) H4B(0.5)
8.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B),
 C78A(H78D,H78E,H78F)
8.b Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C29(H29), C30(H30), C30(H30A), C43(H43), C44(H44),
 C57(H57), C57(H57A), C58(H58)
8.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)
8.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), C38A(H38A), C39A(H39A), C40A(H40A), C41A(H41A),
 C42A(H42A), C60A(H60A), C61A(H61A), C62A(H62A), C63A(H63A), C64A(H64A)
8.e Fitted hexagon refined as free rotating group:
 C37(C38,C39,C40,C41,C42), C59(C60,C61,C62,C63,C64), C59A(C60A,C61A,C62A,C63A,
 C64A)
8.f Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C78(H78A,H78B,H78C), C76A(H76A,H76B,
 H76C), C74A(H74D,H74E,H74F)
;
_shelx_res_checksum              77412
_shelx_hkl_checksum              53602
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU