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_7237866
_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 Ho N4 O17'
_chemical_formula_sum            'C58 H32 Cu2 F42 Ho N4 O17'
_chemical_formula_weight         2146.91
_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                74.64(3)
_cell_angle_beta                 85.46(3)
_cell_angle_gamma                87.11(3)
_cell_formula_units_Z            2
_cell_length_a                   12.206(2)
_cell_length_b                   16.503(3)
_cell_length_c                   20.893(4)
_cell_measurement_reflns_used    8937
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.9064
_cell_measurement_theta_min      1.4092
_cell_volume                     4043.6(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0745
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            39268
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         1.280
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple-green
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             2094
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.487
_refine_diff_density_min         -1.755
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         14259
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1570P)^2^+19.9667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2359
_refine_ls_wR_factor_ref         0.2569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11281
_reflns_number_total             14259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9tc02410g2.cif
_cod_data_source_block           1_CCDC1
_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               7237866
_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
4. Uiso/Uaniso restraints and constraints
F27A \\sim C48: within 2A 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              59747
_shelx_fab_checksum              41273
_olex2_submission_special_instructions 'No special instructions were received'