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_7706086
_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 F36 N5 O17 Tb2, C40 H34 F18 N5 O10 Tb, CHCl3'
_chemical_formula_sum            'C96 H74 Cl3 F54 N10 O27 Tb3'
_chemical_formula_weight         3408.71
_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                95.56(3)
_cell_angle_beta                 106.86(3)
_cell_angle_gamma                105.57(3)
_cell_formula_units_Z            2
_cell_length_a                   14.460(3)
_cell_length_b                   19.762(4)
_cell_length_c                   24.510(5)
_cell_measurement_reflns_used    11603
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8984
_cell_measurement_theta_min      1.8932
_cell_volume                     6340(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0725
_diffrn_reflns_av_unetI/netI     0.1043
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       -29
_diffrn_reflns_number            54406
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.893
_exptl_absorpt_coefficient_mu    1.804
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       block
_exptl_crystal_F_000             3220
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;
TITL Tb in P-1 #2
CELL   14.4600   19.7620   24.5100     95.56    106.86    105.57
SPGR P-1
Q101 0.920 0.908 0.167 !       6.10 eA-3
C102 0.500 1.000 0.000 !       1.53 eA-3
Q103 0.617 0.766 0.266 !       1.26 eA-3
Q104 0.537 0.783 0.008 !       1.14 eA-3
C105 0.533 0.438 0.012 !       1.11 eA-3
Q106 0.140 0.075 0.384 !       1.05 eA-3
C107 0.452 0.927 0.007 !       1.03 eA-3
Q108 0.063 0.295 0.313 !       1.01 eA-3
Q109 0.657 0.566 0.088 !       1.01 eA-3
Q110 0.559 0.299 0.049 !       1.00 eA-3
Q111 0.032 0.110 0.003 !       1.00 eA-3
Q112 0.595 0.235 0.150 !       0.99 eA-3
Q113 0.904 0.780 0.140 !       0.98 eA-3
C114 0.599 0.012 0.077 !       0.98 eA-3
Q115 0.970 0.454 0.010 !       0.97 eA-3
Q116 0.981 0.203 0.239 !       0.97 eA-3
Q117 0.637 0.970 0.256 !       0.97 eA-3
C118 0.529 0.998 0.077 !       0.95 eA-3
C119 0.517 0.526 0.059 !       0.95 eA-3
C120 0.565 0.985 0.108 !       0.94 eA-3
C121 0.268 0.296 0.482 !       0.94 eA-3
Q122 0.309 0.364 0.043 !       0.94 eA-3
Q123 0.330 0.223 0.476 !       0.93 eA-3
Q124 0.065 0.841 0.420 !       0.93 eA-3
C125 0.282 0.253 0.480 !       0.93 eA-3
Q126 0.609 0.502 0.012 !       0.92 eA-3
C127 0.600 0.467 0.048 !       0.92 eA-3
Q128 0.797 0.360 0.096 !       0.92 eA-3
C129 0.581 0.045 0.069 !       0.92 eA-3
Q130 0.129 0.469 0.129 !       0.91 eA-3
Q131 0.945 0.096 0.350 !       0.91 eA-3
Q132 1.005 0.797 0.444 !       0.91 eA-3
Q133 0.954 0.813 0.204 !       0.90 eA-3
Q134 0.715 0.948 0.063 !       0.89 eA-3
Q135 0.375 0.404-0.002 !       0.89 eA-3
C136 0.585 0.987 0.024 !       0.89 eA-3
Q137 0.581 0.296 0.174 !       0.88 eA-3
Q138 0.565 0.795 0.280 !       0.88 eA-3
Q139 0.546 0.940 0.080 !       0.88 eA-3
Q140 0.516 0.324 0.070 !       0.88 eA-3
Q141 0.359 0.079 0.106 !       0.88 eA-3
Q142 0.730 0.888 0.121 !       0.87 eA-3
Q143 0.471 0.066 0.174 !       0.87 eA-3
Q144 0.626 0.564 0.405 !       0.87 eA-3
Q145 0.171 0.114 0.300 !       0.87 eA-3
C146 0.449 0.970 0.015 !       0.87 eA-3
Q147 0.146 0.093 0.308 !       0.86 eA-3
Q148 0.502 0.688 0.025 !       0.86 eA-3
Q149 0.537 0.092 0.069 !       0.86 eA-3
C150 0.644 0.140 0.055 !       0.86 eA-3
Q151 0.391 0.544 0.011 !       0.86 eA-3
Q152 0.126 0.782 0.015 !       0.85 eA-3
Q153 0.546 0.597 0.336 !       0.85 eA-3
Q154 0.596 0.422 0.068 !       0.85 eA-3
Q155 0.331 0.172 0.448 !       0.85 eA-3
Q156 0.357 0.842 0.430 !       0.85 eA-3
Q157 0.738 0.047 0.266 !       0.85 eA-3
Q158 0.144 0.709 0.429 !       0.85 eA-3
Q159 0.704 0.403 0.003 !       0.84 eA-3
Q160 0.096 0.376 0.079 !       0.84 eA-3
Q161 0.045 0.437 0.217 !       0.84 eA-3
Q162 1.003 0.934 0.140 !       0.84 eA-3
Q163 0.673 0.798 0.187 !       0.84 eA-3
Q164 0.377 0.673 0.357 !       0.84 eA-3
Q165 0.044 0.924 0.223 !       0.83 eA-3
Q166 0.312 0.125 0.483 !       0.83 eA-3
Q167 0.429 0.091 0.005 !       0.83 eA-3
Q168 0.802 0.278 0.027 !       0.83 eA-3
C169 0.297 0.315 0.448 !       0.83 eA-3
Q170 0.675 0.224 0.052 !       0.83 eA-3
Q171 0.629 0.435 0.428 !       0.82 eA-3
Q172 0.624 0.611 0.075 !       0.82 eA-3
Q173 0.449 0.408 0.469 !       0.82 eA-3
Q174 0.015 0.250 0.397 !       0.82 eA-3
Q175 0.393 0.735 0.008 !       0.82 eA-3
Q176 0.407 0.387 0.016 !       0.82 eA-3
Q177 0.154 0.299 0.423 !       0.81 eA-3
Q178 0.752 0.467 0.295 !       0.81 eA-3
C179 0.512 0.998 0.045 !       0.81 eA-3
Q180 0.355 0.281 0.439 !       0.81 eA-3
C181 0.637 0.174 0.018 !       0.81 eA-3
C182 0.282 0.229 0.444 !       0.81 eA-3
C183 0.505 0.021 0.041 !       0.81 eA-3
Q184 0.769 0.373 0.114 !       0.81 eA-3
C185 0.692 0.360 0.077 !       0.81 eA-3
C186 0.516 0.527 0.014 !       0.81 eA-3
Q187 0.228 0.034 0.366 !       0.81 eA-3
Q188 0.937 0.925 0.225 !       0.80 eA-3
C189 0.518 0.482 0.029 !       0.80 eA-3
Q190 0.891 0.892 0.046 !       0.80 eA-3
Q191 0.281 0.355 0.439 !       0.80 eA-3
Q192 0.943 0.782 0.256 !       0.79 eA-3
Q193 0.063 0.830 0.397 !       0.79 eA-3
Q194 0.783 0.307 0.064 !       0.79 eA-3
Q195 0.779 0.173 0.328 !       0.79 eA-3
C196 0.440 0.595 0.043 !       0.79 eA-3
Q197 0.330 0.018 0.272 !       0.79 eA-3
Q198 0.669 0.840 0.153 !       0.79 eA-3
Q199 0.597 0.720 0.403 !       0.79 eA-3
;
_refine_diff_density_max         4.052
_refine_diff_density_min         -3.504
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1719
_refine_ls_number_reflns         22301
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1874
_refine_ls_wR_factor_ref         0.2153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15545
_reflns_number_total             22301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03312j2.cif
_cod_data_source_block           tb
_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_formula_sum        'C96 H74 F54 N10 O27 Tb3 Cl3'
_cod_database_code               7706086
_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
 C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F18, C31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C31) \\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'