Slow relaxation of magnetization in lanthanide-biradical complexes based on a functionalized nitronyl nitroxide biradical.
Sun, Juan; Wu, Qi; Lu, Jiao; Jing, Pei; Du, Yeshuang; Li, Licun; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17414–17420; doi:10.1039/d0dt03312j

data_7706087
_publ_section_title
;
 Slow relaxation of magnetization in lanthanide-biradical complexes based
 on a functionalized nitronyl nitroxide biradical.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17414
_journal_page_last               17420
_journal_paper_doi               10.1039/d0dt03312j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C55 H39 Dy2 F36 N5 O17, C40 H34 Dy F18 N5 O10, CHCl3'
_chemical_formula_sum            'C96 H74 Cl3 Dy3 F54 N10 O27'
_chemical_formula_weight         3419.44
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2020-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-21 deposited with the CCDC.	2020-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                95.37(3)
_cell_angle_beta                 107.02(3)
_cell_angle_gamma                105.55(3)
_cell_formula_units_Z            2
_cell_length_a                   14.509(3)
_cell_length_b                   19.777(4)
_cell_length_c                   24.544(5)
_cell_measurement_reflns_used    11267
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8346
_cell_measurement_theta_min      1.5035
_cell_volume                     6374(3)
_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  0.1149
_diffrn_reflns_av_unetI/netI     0.1502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61343
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.503
_exptl_absorpt_coefficient_mu    1.889
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             3226
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
TITL Dy in P-1 #2
CELL   14.5090   19.7770   24.5440     95.37    107.02    105.55
SPGR P-1
Q101 0.580 0.594 0.333 !       3.20 eA-3
C102 0.217 0.201 0.008 !       1.93 eA-3
Q103 0.418 0.972 0.483 !       1.93 eA-3
Q104 0.542 0.217 0.125 !       1.82 eA-3
Q105 0.346 0.768 0.022 !       1.80 eA-3
Q106 0.233 0.372 0.476 !       1.79 eA-3
C107 0.075 0.502 0.502 !       1.78 eA-3
Q108 0.814 0.509 0.458 !       1.75 eA-3
C109 0.948 0.045 0.484 !       1.74 eA-3
C110 0.027 0.502 0.461 !       1.73 eA-3
C111 0.849 0.109 0.445 !       1.73 eA-3
Q112 0.776 0.124 0.458 !       1.72 eA-3
Q113 0.988 0.010 0.421 !       1.72 eA-3
Q114 0.922 0.483 0.046 !       1.71 eA-3
Q115 0.565 0.139 0.422 !       1.69 eA-3
Q116 0.989 0.936 0.429 !       1.67 eA-3
C117 0.124 0.562 0.491 !       1.67 eA-3
Q118 0.192 0.454 0.462 !       1.66 eA-3
C119 0.799 0.137 0.412 !       1.66 eA-3
Q120 0.900 0.097 0.427 !       1.66 eA-3
C121 0.279 0.266 0.086 !       1.65 eA-3
Q122 0.130 0.904 0.156 !       1.65 eA-3
Q123 0.876 0.563 0.460 !       1.63 eA-3
Q124 0.233 0.423 0.489 !       1.62 eA-3
Q125 0.908 0.299 0.467 !       1.62 eA-3
C126 0.263 0.233 0.043 !       1.61 eA-3
C127 0.860 0.317 0.475 !       1.59 eA-3
Q128 0.082 0.420 0.404 !       1.58 eA-3
Q129 0.795 0.347 0.467 !       1.57 eA-3
C130 0.982 0.066 0.446 !       1.55 eA-3
C131 0.059 0.971 0.467 !       1.53 eA-3
C132 0.951 0.421 0.496 !       1.53 eA-3
Q133 0.969 0.158 0.480 !       1.53 eA-3
Q134 0.940 0.360 0.496 !       1.53 eA-3
C135 0.064 0.517 0.433 !       1.51 eA-3
Q136 0.199 0.364 0.432 !       1.50 eA-3
Q137 0.796 0.734 0.018 !       1.49 eA-3
C138 0.957 0.999 0.455 !       1.48 eA-3
Q139 0.957 0.248 0.476 !       1.47 eA-3
Q140 0.990 0.130 0.497 !       1.47 eA-3
Q141 0.892 0.723 0.482 !       1.46 eA-3
C142 0.982 0.421 0.486 !       1.46 eA-3
Q143 0.474 0.112 0.290 !       1.46 eA-3
Q144 0.796 0.299 0.459 !       1.45 eA-3
Q145 0.076 0.938 0.158 !       1.44 eA-3
Q146 0.733 0.266 0.132 !       1.44 eA-3
Q147 0.452 0.672 0.073 !       1.44 eA-3
C148 0.251 0.268 0.018 !       1.44 eA-3
Q149 0.914 0.144 0.479 !       1.43 eA-3
C150 0.122 0.470 0.447 !       1.43 eA-3
C151 0.891 0.981 0.460 !       1.40 eA-3
C152 0.056 0.015 0.490 !       1.40 eA-3
Q153 0.751 0.091 0.421 !       1.40 eA-3
Q154 0.527 0.985 0.335 !       1.39 eA-3
Q155 0.234 0.489 0.500 !       1.39 eA-3
C156 0.915 0.120 0.487 !       1.39 eA-3
Q157 0.952 0.499 0.008 !       1.38 eA-3
C158 0.016 0.124 0.467 !       1.38 eA-3
C159 0.969 0.516 0.398 !       1.38 eA-3
Q160 0.520 0.175 0.439 !       1.36 eA-3
Q161 0.888 0.204 0.483 !       1.36 eA-3
Q162 0.420 0.047 0.267 !       1.36 eA-3
Q163 0.138 0.173 0.008 !       1.36 eA-3
C164 0.081 0.950 0.427 !       1.36 eA-3
C165 0.026 0.067 0.493 !       1.35 eA-3
C166 0.966 0.549 0.377 !       1.35 eA-3
Q167 0.077 0.047 0.049 !       1.34 eA-3
Q168 0.954 0.392 0.422 !       1.34 eA-3
Q169 0.173 0.313 0.069 !       1.33 eA-3
C170 0.954 0.924 0.462 !       1.33 eA-3
Q171 0.361 0.654 0.117 !       1.33 eA-3
Q172 0.866 0.451 0.463 !       1.32 eA-3
C173 0.222 0.292 0.036 !       1.31 eA-3
C174 0.984 0.487 0.492 !       1.31 eA-3
Q175 0.832 0.482 0.494 !       1.31 eA-3
Q176 0.044 1.005 0.433 !       1.31 eA-3
Q177 0.734 0.188 0.258 !       1.30 eA-3
C178 0.980 0.912 0.461 !       1.30 eA-3
Q179 0.110 0.955 0.243 !       1.30 eA-3
Q180 0.295 0.208 0.027 !       1.30 eA-3
Q181 0.877 0.612 0.483 !       1.30 eA-3
Q182 0.465 0.310 0.071 !       1.29 eA-3
Q183 0.705 0.223 0.474 !       1.28 eA-3
Q184 0.126 0.248-0.003 !       1.28 eA-3
Q185 0.904 0.237 0.418 !       1.28 eA-3
Q186 0.296 0.190 0.088 !       1.28 eA-3
Q187 0.926 0.595 0.438 !       1.28 eA-3
Q188 0.969 0.499 0.092 !       1.28 eA-3
Q189 0.467 0.234 0.097 !       1.27 eA-3
Q190 0.609 0.029 0.484 !       1.26 eA-3
Q191 0.826 0.579 0.011 !       1.26 eA-3
C192 0.072 0.613 0.470 !       1.26 eA-3
Q193 0.983 0.678 0.446 !       1.26 eA-3
Q194 0.999 0.797 0.431 !       1.26 eA-3
Q195 0.610 0.232 0.394 !       1.26 eA-3
Q196 0.172 0.465 0.424 !       1.26 eA-3
C197 0.784 0.076 0.458 !       1.26 eA-3
Q198 0.951 0.592 0.494 !       1.25 eA-3
Q199 0.640 0.532 0.375 !       1.25 eA-3
;
_refine_diff_density_max         2.096
_refine_diff_density_min         -2.762
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1719
_refine_ls_number_reflns         22460
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      2.708
_refine_ls_R_factor_all          0.1612
_refine_ls_R_factor_gt           0.1177
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1112P)^2^+54.2133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2695
_refine_ls_wR_factor_ref         0.3055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15451
_reflns_number_total             22460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03312j2.cif
_cod_data_source_block           dy
_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/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        6373(3)
_cod_original_formula_sum        'C96 H74 Dy3 F54 N10 O27 Cl3'
_cod_database_code               7706087
_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. Rigid bond restraints
 F6, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
Uanis(F14) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C35) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F16)
\\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(F8) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
4.a Rotating group:
 O17(H17A,H17B)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C25(H25), C24(H24), C22(H22), C23(H23), C13(H13), C28(H28),
 C48(H48), C43(H43), C53(H53), C33(H33), C77(H77), C66(H66), C64(H64), C68(H68),
  C78(H78), C80(H80), C79(H79), C93(H93), C88(H88), C83(H83), C38(H38)
4.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C20(H20A,H20B,H20C),
 C17(H17C,H17D,H17E), C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C),
  C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C71(H71A,H71B,
 H71C), C61(H61A,H61B,H61C), C58(H58A,H58B,H58C), C57(H57A,H57B,H57C), C60(H60A,
 H60B,H60C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'