Modulating the magnetization dynamics in Ln-Cu-Rad hetero-tri-spin complexes through <i>cis</i>/<i>trans</i> coordination of nitronyl nitroxide radicals around the metal center.
Lu, Jiao; Jing, Pei; Jin, Chaoyi; Xie, Junfang; Li, Licun; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3280–3288; doi:10.1039/d1dt00090j

data_7706574
_publ_section_title
;
 Modulating the magnetization dynamics in Ln-Cu-Rad hetero-tri-spin
 complexes through <i>cis</i>/<i>trans</i> coordination of nitronyl
 nitroxide radicals around the metal center.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3280
_journal_page_last               3288
_journal_paper_doi               10.1039/d1dt00090j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C61 H45 Cu Dy F30 N6 O14'
_chemical_formula_sum            'C61 H45 Cu Dy F30 N6 O14'
_chemical_formula_weight         1882.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc26ybq7
_audit_creation_date             2020-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2021-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.350(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4060(4)
_cell_length_b                   20.0653(4)
_cell_length_c                   17.4861(3)
_cell_measurement_reflns_used    22165
_cell_measurement_temperature    80
_cell_measurement_theta_max      73.3250
_cell_measurement_theta_min      4.0690
_cell_volume                     7147.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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      80
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35073
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.642
_diffrn_reflns_theta_min         3.916
_exptl_absorpt_coefficient_mu    7.215
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70977
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       prism
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.516
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         13276
_refine_ls_number_restraints     332
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.1060
_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^)+(0.0400P)^2^+200.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12291
_reflns_number_total             13276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00090j2.cif
_cod_data_source_block           lj-dycu_pl
_cod_depositor_comments
'Adding full bibliography for 7706571--7706575.cif.'
_cod_database_code               7706574
_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
 C44-C45
 1.5 with sigma of 0.02
 C45-O8
 1.2 with sigma of 0.01
 F24-F23
 1.8 with sigma of 0.01
 F24A-F22
 1.8 with sigma of 0.01
 F16B-F18A
 1.8 with sigma of 0.01
 F20-F19
 1.8 with sigma of 0.01
 F28-F30
 1.8 with sigma of 0.01
 F14-F13
 1.9 with sigma of 0.01
 F9A-F7
 1.8 with sigma of 0.01
 F12-F10A
 1.8 with sigma of 0.01
3. Rigid bond restraints
 F7, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 F30, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 F24, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 O9, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 F19, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C49, C50, O10, C51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F15A, F13, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C56, F23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F16B \\sim F12 \\sim F5 \\sim F14 \\sim F1 \\sim F30 \\sim F11 \\sim F9 \\sim
F18 \\sim F10 \\sim F8 \\sim F6 \\sim F13 \\sim F15 \\sim F24 \\sim F20 \\sim
F21 \\sim F7 \\sim F2 \\sim F19 \\sim F25 \\sim F23 \\sim F29 \\sim F3 \\sim
F17 \\sim F26 \\sim F27 \\sim F4 \\sim F28 \\sim F22: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F18A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F28A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F15A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F10A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(F24A)=1-FVAR(1)
 Sof(F24)=FVAR(1)
 Sof(F18A)=1-FVAR(2)
 Sof(F18)=FVAR(2)
 Sof(F20A)=1-FVAR(3)
 Sof(F20)=FVAR(3)
 Sof(F16C)=1-FVAR(4)
 Sof(F16B)=FVAR(4)
 Sof(F28A)=1-FVAR(5)
 Sof(F28)=FVAR(5)
 Sof(F9A)=1-FVAR(6)
 Sof(F9)=FVAR(6)
 Sof(F15A)=1-FVAR(7)
 Sof(F15)=FVAR(7)
 Sof(F10A)=1-FVAR(8)
 Sof(F10)=FVAR(8)
6.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C14(H14), C39(H39), C34(H34), C54(H54), C30(H30), C49(H49),
 C28(H28), C27(H27), C35(H35), C32(H32), C33(H33), C36(H36), C9(H9), C44(H44),
 C12(H12), C10(H10), C59(H59), C15(H15), C16(H16), C18(H18)
6.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C),
 C4(H4A,H4B,H4C), C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              14883
_shelx_hkl_checksum              77956
_olex2_submission_special_instructions 'No special instructions were received'