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_7059631
_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 Mn4 N5 O43 Y4, N O3'
_chemical_formula_sum            'C74 H123 Mn4 N9 O56 Y4'
_chemical_formula_weight         2610.21
_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                79.398(3)
_cell_angle_beta                 69.241(2)
_cell_angle_gamma                76.963(3)
_cell_formula_units_Z            2
_cell_length_a                   16.9322(5)
_cell_length_b                   18.8267(6)
_cell_length_c                   19.8169(6)
_cell_measurement_reflns_used    18438
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.46
_cell_measurement_theta_min      3.06
_cell_volume                     5717.2(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.951
_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  0.0842
_diffrn_reflns_av_unetI/netI     0.1104
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52554
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.921
_diffrn_reflns_theta_min         3.058
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    6.889
_exptl_absorpt_correction_T_max  0.5297
_exptl_absorpt_correction_T_min  0.1036
_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_colour_primary    brown
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2668
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1211
_refine_ls_number_reflns         20591
_refine_ls_number_restraints     691
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1722
_refine_ls_R_factor_gt           0.0976
_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^)+(0.1762P)^2^+3.7067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2582
_refine_ls_wR_factor_ref         0.3109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10594
_reflns_number_total             20591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01517b2.cif
_cod_data_source_block           Y4Mn4
_cod_depositor_comments
;Adding full bibliography for 7059628--7059633.cif.

 Adding full bibliography for 7059628--7059633.cif.
;
_cod_database_code               7059631
_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
 C48-C49
 2.5 with sigma of 0.02
 O19-C47 = C46-C47 = C48-C46 = O20-C48 = C49-C46 = C49-C50 = C46-C45
 1.5 with sigma of 0.02
 C49-O20
 3 with sigma of 0.02
 C49-O19
 3 with sigma of 0.02
 C49-C45
 3 with sigma of 0.02
 C48-C47
 2.5 with sigma of 0.02
 C37-C38 = C34-C37 = C34-C36 = O12-C36 = C34-C35 = C33-C34 = O8-C30 = C30-C28 =
  C29-C28 = O7-C29 = C31-C28 = C31-C32 = C44-C43 = C43-C40 = C40-C39 = O16-C41 =
  C42-C40 = O15-C42 = C40-C41
 1.5 with sigma of 0.02
 O11-C35 = O12-C36 = O7-C29
 1.4 with sigma of 0.02
3. Rigid bond restraints
 C26, C25, N5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O9 \\sim O10 \\sim O11 \\sim O12 \\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 O6 \\sim O7 \\sim O8 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31
\\sim C32: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O17 \\sim O18 \\sim O19 \\sim O20 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C49 \\sim C50: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
O37 \\sim O38 \\sim O39 \\sim N6: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
O13 \\sim O14 \\sim O15 \\sim O16 \\sim C39 \\sim C41 \\sim C42 \\sim C43 \\sim
C44: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C4 \\sim C3 \\sim C2 \\sim C1 \\sim N1 \\sim C5 \\sim C6 \\sim O1: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
N2 \\sim O2 \\sim C12 \\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
O3 \\sim C18 \\sim C16 \\sim C17 \\sim N3 \\sim C13 \\sim C14 \\sim C15: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O4 \\sim C24 \\sim C23 \\sim N4 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C61 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim O26 \\sim O25 \\sim O28 \\sim
O27 \\sim C62: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C56 \\sim C55 \\sim C53 \\sim C52 \\sim C54 \\sim O24 \\sim O22 \\sim C51 \\sim
O21 \\sim O23: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C68 \\sim C67 \\sim C65 \\sim C64 \\sim C66 \\sim O30 \\sim O32 \\sim C63 \\sim
O31 \\sim O29: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C74 \\sim C73 \\sim O33 \\sim C69 \\sim O34 \\sim C72 \\sim C71 \\sim C70 \\sim
O35 \\sim O36: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
N5 \\sim C25 \\sim C26: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
Uanis(C42) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.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)
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:
 C56(H56A,H56B,H56C), C62(H62A,H62B,H62C), C68(H68A,H68B,H68C), C74(H74A,H74B,
 H74C)
;
_shelx_res_checksum              7912
_shelx_fab_checksum              318
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'