Slow relaxation of magnetization in unprecedented Cu‒Ln-Rad hetero-tri-spin chains constructed from multidentate nitronyl nitroxide
Sun, Juan; Sun, Zan; Wang, Kang; Xi, Lu; Ma, Yue; Li, Licun; Journal of Materials Chemistry C 7 (2019) 9057–; doi:10.1039/C9TC02410G

data_7237865
_publ_section_title
;
 Slow relaxation of magnetization in unprecedented Cu--Ln-Rad
 hetero-tri-spin chains constructed from multidentate nitronyl nitroxide
;
_journal_issue                   29
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              9057
_journal_paper_doi               10.1039/C9TC02410G
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C58 H32 Cu2 F42 Gd N4 O17'
_chemical_formula_sum            'C58 H32 Cu2 F42 Gd N4 O17'
_chemical_formula_weight         2139.23
_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   mixed
_audit_creation_date             2018-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-01 deposited with the CCDC.	2019-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                74.45(3)
_cell_angle_beta                 85.57(3)
_cell_angle_gamma                87.15(3)
_cell_formula_units_Z            2
_cell_length_a                   12.208(2)
_cell_length_b                   16.603(3)
_cell_length_c                   20.871(4)
_cell_measurement_reflns_used    4646
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8704
_cell_measurement_theta_min      1.2737
_cell_volume                     4061.5(14)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.1500
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1240
_diffrn_reflns_av_unetI/netI     0.1739
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38949
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.274
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple-green
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         14255
_refine_ls_number_restraints     1231
_refine_ls_restrained_S_all      1.371
_refine_ls_R_factor_all          0.1731
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1212P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2292
_refine_ls_wR_factor_ref         0.2857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7731
_reflns_number_total             14255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9tc02410g2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7237865
_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, All O(H,H) groups
2. Restrained distances
 F34-O14
 2.8 with sigma of 0.01
 C32A-C31A
 1.53 with sigma of 0.01
3. Rigid bond restraints
 F9A, C38
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O8, C37A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C38
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C35
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C47
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O10, C32A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 F25, F27B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C29, C37B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
F27A \\sim C48: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C44 \\sim C29 \\sim C18 \\sim C57 \\sim C50 \\sim C23 \\sim C9 \\sim C10 \\sim
C14 \\sim C8 \\sim C52 \\sim C13 \\sim C12 \\sim C7 \\sim C17 \\sim C27 \\sim
C19 \\sim C26 \\sim C11 \\sim C16 \\sim C4 \\sim C25 \\sim C6 \\sim C15 \\sim
C40 \\sim C22 \\sim C45 \\sim C1 \\sim C5 \\sim C28 \\sim C20 \\sim C55 \\sim
C42 \\sim C3 \\sim C41 \\sim C24 \\sim C33 \\sim C2 \\sim C58 \\sim C53 \\sim
C51 \\sim C46 \\sim C56 \\sim C54 \\sim C21 \\sim C47 \\sim C39 \\sim C30A
\\sim C35 \\sim C43 \\sim C31A \\sim C37A \\sim C36A \\sim C38 \\sim C32A \\sim
C49 \\sim C30B \\sim C31B \\sim C32B \\sim C37B \\sim C36B \\sim C48 \\sim C34:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F35A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(F35B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C38) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C38) \\sim Ueq, Uanis(F36) \\sim Ueq, Uanis(F9) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
Uanis(F34) \\sim Ueq, Uanis(F36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C36A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(F9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(F42) \\sim Ueq, Uanis(F30) \\sim Ueq, Uanis(C37A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(F40) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C32A) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(O10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(F9A) \\sim Ueq, Uanis(F27B) \\sim Ueq, Uanis(C32B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(C49) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(F9A)=1-FVAR(1)
 Sof(F9)=FVAR(1)
 Fixed Sof: C30A(0.5) C31A(0.5) H31A(0.5) F35B(0.5) F35A(0.5) C37A(0.5)
 C36A(0.5) H36A(0.5) C32A(0.5) C30B(0.5) C31B(0.5) H31B(0.5) C32B(0.5)
 C37B(0.5) C36B(0.5) H36B(0.5) F27A(0.5) F27B(0.5)
6.a Rotating group:
 O11(H11A,H11B)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C23(H23), C9(H9), C13(H13), C17(H17), C26(H26), C11(H11), C16(H16),
 C15(H15), C22(H22), C20(H20), C41(H41), C51(H51), C46(H46), C56(H56), C21(H21),
  C31A(H31A), C36A(H36A), C31B(H31B), C36B(H36B)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              58685
_shelx_fab_checksum              93149
_olex2_submission_special_instructions 'No special instructions were received'