Supramolecular heptanuclear Ln-Cu complexes involving nitronyl nitroxide biradicals: structure and magnetic behavior
Xi, Lu; Jin, Chaoyi; Song, Hong-Wei; Wang, Xiao-Tong; Li, Licun; Sutter, Jean-Pascal; Dalton Transactions  (2022) –; doi:10.1039/D2DT00220E

data_7709991
_publ_section_title
;
 Supramolecular heptanuclear Ln-Cu complexes involving nitronyl nitroxide
 biradicals: structure and magnetic behavior
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00220E
_journal_year                    2022
_chemical_formula_moiety
'2(C47 H34 Cu F30 N7 O14 Tb), C84 H66 Cu F48 N14 O24 Tb2'
_chemical_formula_sum            'C178 H134 Cu3 F108 N28 O52 Tb4'
_chemical_formula_weight         6375.42
_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             2019-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-26 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                85.11(3)
_cell_angle_beta                 71.23(3)
_cell_angle_gamma                85.78(3)
_cell_formula_units_Z            1
_cell_length_a                   14.696(3)
_cell_length_b                   21.242(4)
_cell_length_c                   21.576(4)
_cell_measurement_reflns_used    12418
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.8824
_cell_measurement_theta_min      1.3418
_cell_volume                     6346(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2014)'
_diffrn_ambient_temperature      113
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61509
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.342
_exptl_absorpt_coefficient_mu    1.498
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple-green
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       strip
_exptl_crystal_F_000             3133
_exptl_crystal_size_max          0.2200
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1800
_refine_diff_density_max         2.116
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1677
_refine_ls_number_reflns         22348
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0820
_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^)+(0.1401P)^2^+24.1532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2224
_refine_ls_wR_factor_ref         0.2531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16599
_reflns_number_total             22348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00220e2.cif
_cod_data_source_block           Tb-Cu
_cod_database_code               7709991
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C68-C67
 1.4 with sigma of 0.01
3. Rigid bond restraints
 C20, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C25 \\sim C24 \\sim C26 \\sim O7: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C36(H36), C9(H9), C58(H58), C11(H11), C37(H37), C56(H56), C63(H63),
 C84(H84), C83(H83), C87(H87), C45(H45), C60(H60), C16(H16), C40(H40), C73(H73),
  C21(H21), C68(H68), C26(H26)
5.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C78(H78A,H78B,H78C), C48(H48A,H48B,H48C), C31(H31A,H31B,
 H31C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C51(H51A,H51B,H51C), C32(H32A,H32B,
 H32C), C1(H1A,H1B,H1C), C81(H81A,H81B,H81C), C3(H3A,H3B,H3C), C79(H79A,H79B,
 H79C), C76(H76A,H76B,H76C), C34(H34A,H34B,H34C), C50(H50A,H50B,H50C), C53(H53A,
 H53B,H53C)
;
_shelx_res_checksum              3987
_shelx_hkl_checksum              14967
_shelx_fab_checksum              55113
_olex2_submission_special_instructions 'No special instructions were received'