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_7059632
_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 Dy4 Mn4 N5 O43'
_chemical_formula_sum            'C74 H123 Dy4 Mn4 N9 O56'
_chemical_formula_weight         2904.57
_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                79.081(3)
_cell_angle_beta                 69.234(3)
_cell_angle_gamma                76.840(3)
_cell_formula_units_Z            2
_cell_length_a                   16.9478(7)
_cell_length_b                   18.9017(8)
_cell_length_c                   19.8300(8)
_cell_measurement_reflns_used    21685
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.77
_cell_measurement_theta_min      3.06
_cell_volume                     5742.4(4)
_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 0.967
_diffrn_measured_fraction_theta_max 0.942
_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  0.0785
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            44841
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.011
_diffrn_reflns_theta_min         3.059
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    17.920
_exptl_absorpt_correction_T_max  0.2833
_exptl_absorpt_correction_T_min  0.0439
_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    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2884
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.312
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1269
_refine_ls_number_reflns         20533
_refine_ls_number_restraints     666
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.0932
_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^)+(0.1738P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2462
_refine_ls_wR_factor_ref         0.2903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11034
_reflns_number_total             20533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01517b2.cif
_cod_data_source_block           Dy4Mn4
_cod_depositor_comments
;Adding full bibliography for 7059628--7059633.cif.

 Adding full bibliography for 7059628--7059633.cif.
;
_cod_database_code               7059632
_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
 C41-C38 = C38-C37
 1.5 with sigma of 0.02
 C47-C44 = C48-C47 = C44-C43
 1.5 with sigma of 0.02
 O14-C40 = C40-C38 = C41-C38 = C42-C41 = C38-C37 = O13-C37 = O12-C37
 1.5 with sigma of 0.02
 C45-C44 = O18B-C45 = C47-C44 = C48-C47 = C44-C43 = O16-C43 = O17-C43
 1.5 with sigma of 0.02
 O19B-C46 = O19A-C46 = O18A-C45 = O18B-C45
 1.5 with sigma of 0.02
 O15B-C39 = C39-C38
 1.5 with sigma of 0.02
 O15A-C39
 1.5 with sigma of 0.02
 O11B-C33 = O11A-C33
 1.5 with sigma of 0.02
 O19A-O18A
 2 with sigma of 0.02
 O14-O15B
 2 with sigma of 0.02
 O6A-O7A
 2.5 with sigma of 0.02
 C29A-C30 = C30-C29B = O6A-C27A
 1.5 with sigma of 0.02
 O7A-C28A = C26A-C28A = O7B-C28B = C26B-C28B = O6B-C27A = O6B-C27B = C26B-C27B
 = C26A-C27A = C29A-C26A = C26B-C29B = C26A-C25 = C26B-C25
 1.5 with sigma of 0.02
 C29B-C27B
 2 with sigma of 0.02
 C29B-C27B = O6B-C29B
 2.5 with sigma of 0.02
 O6A-C26A
 2.5 with sigma of 0.02
 O15B-C38
 2.5 with sigma of 0.02
 O14-C40
 1.4 with sigma of 0.02
 C74-C73
 1.5 with sigma of 0.02
 N5-C73
 1.15 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O12 \\sim O13 \\sim O14 \\sim C37 \\sim C38 \\sim C40 \\sim C41 \\sim C42:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O16 \\sim O17 \\sim O18B \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47
\\sim C48: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O16 \\sim O17 \\sim O18A \\sim O18B \\sim O19A \\sim O19B \\sim C43 \\sim C44
\\sim C45 \\sim C46 \\sim C47 \\sim C48: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
O12 \\sim O13 \\sim O14 \\sim O15B \\sim C37 \\sim C38 \\sim C39 \\sim C40
\\sim C41 \\sim C42: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O12 \\sim O13 \\sim O14 \\sim O15A \\sim O15B \\sim C37 \\sim C38 \\sim C39
\\sim C40 \\sim C41 \\sim C42: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
O5 \\sim O6 \\sim C25: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O5 \\sim O6 \\sim O6A \\sim O6B \\sim O7A \\sim O7B \\sim C25 \\sim C26A \\sim
C26B \\sim C27A \\sim C27B \\sim C28A \\sim C28B \\sim C29A \\sim C29B \\sim
C30: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O6A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C24 \\sim C23 \\sim N4 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim O4: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
N5 \\sim C73 \\sim C74: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O2 \\sim C12 \\sim C10 \\sim C11 \\sim N2 \\sim C7 \\sim C8 \\sim C9: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C6 \\sim C4 \\sim C3 \\sim C2 \\sim C1 \\sim N1 \\sim C5 \\sim O1: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
C13 \\sim N3 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim O3: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O8 \\sim O9 \\sim O10 \\sim O11B \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim
C35 \\sim C36: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
O8 \\sim O9 \\sim O10 \\sim O11A \\sim O11B \\sim C31 \\sim C32 \\sim C33 \\sim
C34 \\sim C35 \\sim C36: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
Uanis(O6A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N5) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O18A)=Sof(O19A)=1-FVAR(1)
 Sof(O18B)=Sof(O19B)=FVAR(1)
 Sof(O15A)=1-FVAR(2)
 Sof(O15B)=FVAR(2)
 Sof(O11A)=1-FVAR(3)
 Sof(O11B)=FVAR(3)
 Sof(O6B)=Sof(O7B)=Sof(C26B)=Sof(C27B)=Sof(C28B)=Sof(C29B)=1-FVAR(4)
 Sof(O6A)=Sof(O7A)=Sof(C26A)=Sof(C27A)=Sof(C28A)=Sof(C29A)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C51(H51A,H51B),
 C52(H52A,H52B), C53(H53A,H53B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
  C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C69(H69A,H69B), C70(H70A,
 H70B), C71(H71A,H71B)
5.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)
5.c Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C60(H60A,H60B,H60C), C66(H66A,H66B,H66C), C72(H72A,H72B,
 H72C)
;
_shelx_res_checksum              13176
_shelx_fab_checksum              96686
_olex2_submission_special_instructions 'No special instructions were received'