Syntheses, structures and magnetic properties of novel tetrameric Ln2Mn2 and ring-like Ln4Mn4 clusters
Yin, Jia-Jia; Chen, Cheng; Zhuang, Gui-Lin; Zheng, Jun; Zheng, Xiu-Ying; Shao, Feng; New Journal of Chemistry 44 (2020) 9837–9843; doi:10.1039/D0NJ01517B

data_7059633
_publ_section_title
;
 Syntheses, structures and magnetic properties of novel tetrameric Ln2Mn2
 and ring-like Ln4Mn4 clusters
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9837
_journal_page_last               9843
_journal_paper_doi               10.1039/D0NJ01517B
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C74 H60 Gd4 Mn4 N5 O43'
_chemical_formula_sum            'C74 H123 Gd4 Mn4 N9 O56'
_chemical_formula_weight         2883.57
_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   geom
_audit_creation_date             2020-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-30 deposited with the CCDC.	2020-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                78.846(7)
_cell_angle_beta                 69.215(6)
_cell_angle_gamma                77.089(7)
_cell_formula_units_Z            2
_cell_length_a                   16.9426(14)
_cell_length_b                   18.9636(17)
_cell_length_c                   19.8755(17)
_cell_measurement_reflns_used    25734
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.80
_cell_measurement_theta_min      3.06
_cell_volume                     5773.5(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39369
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        61.499
_diffrn_reflns_theta_max         61.499
_diffrn_reflns_theta_min         3.055
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    18.835
_exptl_absorpt_correction_T_max  0.1873
_exptl_absorpt_correction_T_min  0.0144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.055
_refine_diff_density_min         -1.743
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1296
_refine_ls_number_reflns         17573
_refine_ls_number_restraints     927
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.1118
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2924
_refine_ls_wR_factor_ref         0.3391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10768
_reflns_number_total             17573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01517b2.cif
_cod_data_source_block           Gd4Mn4
_cod_depositor_comments
;Adding full bibliography for 7059628--7059633.cif.

 Adding full bibliography for 7059628--7059633.cif.
;
_cod_database_code               7059633
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C45
 1.5 with sigma of 0.02
 C25A-C26 = C26-C25B
 1.5 with sigma of 0.02
 N5-C25A = N5-C25B
 1.15 with sigma of 0.02
 C50B-C49 = C50A-C49 = C49-C46 = C47-C46 = O19A-C47 = O20B-C48 = C48-C46 =
 O20A-C48 = C46-C45
 1.5 with sigma of 0.02
 O19B-C47
 1.5 with sigma of 0.02
 O19B-O20B
 2.5 with sigma of 0.02
 O15-C40
 2.5 with sigma of 0.02
 O16B-C41B = O15-C42 = C42-C40 = C41B-C40 = C43-C40 = C44-C43 = C40-C39
 1.5 with sigma of 0.02
 O16B-O15
 2.5 with sigma of 0.02
 C41B-C42
 2.5 with sigma of 0.02
 C41A-C40 = O16A-C41A
 1.5 with sigma of 0.02
 C30A-C27
 2.5 with sigma of 0.02
 C30B-C29B
 2.5 with sigma of 0.02
 C29B-C31A
 2.5 with sigma of 0.02
 C29B-C28B
 1.5 with sigma of 0.02
 C28B-C31A
 1.5 with sigma of 0.02
 O7B-C29A = C29A-C30A
 2.5 with sigma of 0.02
 C30B-C28B = O7B-C30B
 1.5 with sigma of 0.02
 C28B-C30A = O7B-C30A
 1.5 with sigma of 0.02
 O8B-C28B
 2.5 with sigma of 0.02
 O8B-C31B = C31B-C28B
 1.5 with sigma of 0.02
 O8A-C31A = C28A-C31A = O7A-C30A = C28A-C30A
 1.5 with sigma of 0.02
 O8A-C30A = C30A-C31A
 2.5 with sigma of 0.02
 C28A-C29A
 1.5 with sigma of 0.02
 C29B-C31B
 2.5 with sigma of 0.02
 C42-C43
 2.5 with sigma of 0.02
 O16B-C42
 2.5 with sigma of 0.02
 C41B-C39
 2.5 with sigma of 0.02
 O15-C42
 1.4 with sigma of 0.02
 C29B-C32
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C38, C37, C36, O11, O10, C33, O9, C34, C35, O12B, O12A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O13, O14, O15, O16A, O16B, C39, C40, C41A, C41B, C42, C43, C44
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O17 \\sim O18 \\sim C45 \\sim C46: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
O13 \\sim O14 \\sim C39: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O5 \\sim O6 \\sim C27: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O9 \\sim O10 \\sim O11 \\sim O12B \\sim C33 \\sim C34 \\sim C35 \\sim C36:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
N5 \\sim C25A \\sim C25B \\sim C26: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
O17 \\sim O18 \\sim O19A \\sim O20A \\sim O20B \\sim C45 \\sim C46 \\sim C47
\\sim C48 \\sim C49 \\sim C50A \\sim C50B: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
O17 \\sim O18 \\sim O19A \\sim O19B \\sim O20A \\sim O20B \\sim C45 \\sim C46
\\sim C47 \\sim C48 \\sim C49 \\sim C50A \\sim C50B: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
O13 \\sim O14 \\sim O15 \\sim O16B \\sim C39 \\sim C40 \\sim C41B \\sim C42
\\sim C43 \\sim C44: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O13 \\sim O14 \\sim O15 \\sim O16A \\sim O16B \\sim C39 \\sim C40 \\sim C41A
\\sim C41B \\sim C42 \\sim C43 \\sim C44: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
O4 \\sim C24: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
N4 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim O4: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O3 \\sim N3 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O2 \\sim C12 \\sim N2 \\sim C11 \\sim C10 \\sim C9 \\sim C8 \\sim C7: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim N3 \\sim O3: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O28 \\sim C59 \\sim C58 \\sim C60 \\sim O27 \\sim C57 \\sim C61 \\sim C62 \\sim
O25 \\sim O26: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C56 \\sim C55 \\sim C53 \\sim O23 \\sim C54 \\sim C52 \\sim O24 \\sim O22 \\sim
C51 \\sim O21: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C74 \\sim C73 \\sim C69 \\sim O33 \\sim O34 \\sim C70 \\sim C72 \\sim C71 \\sim
O35 \\sim O36: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
O9 \\sim O10 \\sim O11 \\sim O12A \\sim O12B \\sim C33 \\sim C34 \\sim C35
\\sim C36 \\sim C37 \\sim C38: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
O5 \\sim O7B \\sim C27 \\sim C28B \\sim C29A \\sim C29B \\sim C30A \\sim C30B
\\sim C32: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O5 \\sim O6 \\sim O7B \\sim C27 \\sim C28B \\sim C29A \\sim C29B \\sim C30A
\\sim C30B \\sim C31A \\sim C32: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
O5 \\sim O6 \\sim O7A \\sim O7B \\sim O8A \\sim O8B \\sim C27 \\sim C28A \\sim
C28B \\sim C29A \\sim C29B \\sim C30A \\sim C30B \\sim C31A \\sim C31B \\sim
C32: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C26) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C25B) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O16B) \\sim Ueq, Uanis(C41B) \\sim Ueq, Uanis(O16A) \\sim Ueq,
Uanis(C41A) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C56) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(O12A)=1-FVAR(1)
 Sof(O12B)=FVAR(1)
 Sof(O19B)=Sof(O20B)=Sof(C25A)=Sof(C50A)=1-FVAR(2)
 Sof(O19A)=Sof(O20A)=Sof(C25B)=Sof(C50B)=FVAR(2)
 Sof(O16A)=Sof(C41A)=1-FVAR(3)
 Sof(O16B)=Sof(C41B)=FVAR(3)
 Sof(O7B)=Sof(O8B)=Sof(C28B)=Sof(C29B)=Sof(C30B)=Sof(C31B)=1-FVAR(4)
 Sof(O7A)=Sof(O8A)=Sof(C28A)=Sof(C29A)=Sof(C30A)=Sof(C31A)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C53(H53A,H53B),
 C54(H54A,H54B), C55(H55A,H55B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B),
  C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C71(H71A,H71B), C72(H72A,
 H72B), C73(H73A,H73B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22)
6.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C62(H62A,H62B,H62C), C68(H68A,H68B,H68C), C74(H74A,H74B,
 H74C)
;
_shelx_res_checksum              91960
_shelx_fab_checksum              98413
_olex2_submission_special_instructions 'No special instructions were received'