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_7059629
_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
'C18 H18 Gd Mn N5 O11, C18 H17 Gd Mn N5 O11, 2(Cl O4), 3(O)'
_chemical_formula_sum            'C36 H50 Cl2 Gd2 Mn2 N10 O33'
_chemical_formula_weight         1646.14
_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             2019-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-09 deposited with the CCDC.	2020-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                98.204(4)
_cell_angle_beta                 99.148(4)
_cell_angle_gamma                98.362(3)
_cell_formula_units_Z            2
_cell_length_a                   14.4122(6)
_cell_length_b                   14.3812(6)
_cell_length_c                   14.5701(7)
_cell_measurement_reflns_used    6420
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.73
_cell_measurement_theta_min      4.01
_cell_volume                     2906.9(2)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.1372
_diffrn_reflns_av_unetI/netI     0.1539
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24441
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        63.991
_diffrn_reflns_theta_max         63.991
_diffrn_reflns_theta_min         3.153
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    19.726
_exptl_absorpt_correction_T_max  0.7121
_exptl_absorpt_correction_T_min  0.1140
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.922
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         9414
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.2086
_refine_ls_R_factor_gt           0.1121
_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^)+(0.1737P)^2^+37.4060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2685
_refine_ls_wR_factor_ref         0.3459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4673
_reflns_number_total             9414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01517b2.cif
_cod_data_source_block           Gd2Mn2
_cod_depositor_comments
;Adding full bibliography for 7059628--7059633.cif.

 Adding full bibliography for 7059628--7059633.cif.
;
_cod_database_code               7059629
_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
2. Restrained distances
 Cl05-O21 = Cl05-O22 = Cl05-O20 = Cl05-O19
 1.5 with sigma of 0.02
 O20-O19
 2 with sigma of 0.02
 O24-O23 \\sim O26-O25
 with sigma of 0.02
 O21-O19 \\sim O20-O22
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl06 \\sim O23 \\sim O24 \\sim O25 \\sim O26: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
Cl05 \\sim O19 \\sim O20 \\sim O21 \\sim O22: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
O10 \\sim N6 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C11 \\sim C10 \\sim C9 \\sim C8 \\sim C7 \\sim N2 \\sim C12 \\sim O2: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C16 \\sim C15 \\sim C14 \\sim C13 \\sim N3 \\sim C17 \\sim C18 \\sim O3: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C35 \\sim C36 \\sim N8 \\sim O12 \\sim C34 \\sim C33 \\sim C32 \\sim C31:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C25 \\sim C29 \\sim N7 \\sim O11 \\sim C30 \\sim C28 \\sim C26 \\sim C27:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O17 \\sim O18 \\sim N10 \\sim O16: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
O5 \\sim N4 \\sim O4 \\sim O6: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B)
4.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), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36)
;
_shelx_res_checksum              50855
_shelx_fab_checksum              19750
_olex2_submission_special_instructions 'No special instructions were received'