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_7709992
_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 Dy F30 N7 O14), C84 H66 Cu Dy2 F48 N14 O24'
_chemical_formula_sum            'C178 H134 Cu3 Dy4 F108 N28 O52'
_chemical_formula_weight         6389.74
_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             2022-03-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_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                 71.25(3)
_cell_angle_gamma                85.82(3)
_cell_formula_units_Z            1
_cell_length_a                   14.789(3)
_cell_length_b                   21.301(4)
_cell_length_c                   21.621(4)
_cell_measurement_reflns_used    13478
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.9103
_cell_measurement_theta_min      1.3383
_cell_volume                     6419(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      113.0
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0813
_diffrn_reflns_av_unetI/netI     0.1080
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_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            51809
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.429
_exptl_absorpt_coefficient_mu    1.544
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6568
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic bluish violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       plank
_exptl_crystal_F_000             3137
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.009
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1685
_refine_ls_number_reflns         21888
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0980
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1181P)^2^+62.3156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2488
_refine_ls_wR_factor_ref         0.2754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15948
_reflns_number_total             21888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00220e2.cif
_cod_data_source_block           Dy-Cu
_cod_original_cell_volume        6419(3)
_cod_database_code               7709992
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.728
_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
 C25-C26
 1.46 with sigma of 0.01
 C20-C21
 1.46 with sigma of 0.01
 C21-C22
 1.46 with sigma of 0.01
 C68-C67
 1.46 with sigma of 0.01
 C27-C26 = C26-C25 = C22-C21 = C21-C20 = C16-C15 = C17-C16 = C88-C87 = C87-C86
 = C45-C44 = C46-C45 = C41-C40 = C40-C39 = C63-C62 = C64-C63 = C68-C67 = C69-
 C68 = C74-C73 = C73-C72
 1.47 with sigma of 0.01
 C52-C51 = C53-C52 = C49-C48 = C50-C49 = C77-C76 = C78-C77 = C80-C79 = C81-C80
 = C2-C1 = C3-C2 = C6-C5 = C5-C4 = C31-C30 = C30-C29 = C33-C32 = C34-C33
 1.5 with sigma of 0.01
 C86-C85 = C89-C88 = C39-C38 = C42-C41 = C47-C46 = C44-C43 = C15-C14 = C18-C17
 = C28-C27 = C25-C24 = C23-C22 = C20-C19 = C62-C61 = C65-C64 = C67-C66 = C70-
 C69 = C72-C71 = C75-C74
 1.53 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
 C25, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C67, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C22, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C75, F47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C25, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 F14, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F11, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F43, C71
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C73 \\sim C72 \\sim C74: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C21 \\sim C20 \\sim C22: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C26 \\sim C25 \\sim C27: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C71) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C58(H58), C13(H13), C11(H11), C9(H9), C37(H37), C56(H56), C63(H63),
 C84(H84), C83(H83), C87(H87), C45(H45), C60(H60), C16(H16), C40(H40), C73(H73),
  C21(H21), C26(H26), C68(H68)
5.b Fitted hexagon refined as free rotating group:
 C8(C13,C12,C11,C10,C9)
5.c 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              4149
_shelx_hkl_checksum              29448
_shelx_fab_checksum              78017
_olex2_submission_special_instructions 'No special instructions were received'