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_7706085
_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 Gd2 N5 O17, C40 H34 F18 Gd N5 O10, CHCl3'
_chemical_formula_sum            'C96 H74 Cl3 F54 Gd3 N10 O27'
_chemical_formula_weight         3403.69
_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             2018-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-20 deposited with the CCDC.	2020-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                75.63(3)
_cell_angle_beta                 72.85(3)
_cell_angle_gamma                74.42(3)
_cell_formula_units_Z            2
_cell_length_a                   14.517(3)
_cell_length_b                   19.785(4)
_cell_length_c                   24.597(5)
_cell_measurement_reflns_used    13059
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8944
_cell_measurement_theta_min      1.5019
_cell_volume                     6392(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0687
_diffrn_reflns_av_unetI/netI     0.0972
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            75460
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.834
_diffrn_reflns_theta_min         1.502
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       block
_exptl_crystal_F_000             3214
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.779
_refine_diff_density_min         -2.194
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1718
_refine_ls_number_reflns         30144
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      4.065
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.035
_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^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20846
_reflns_number_total             30144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03312j2.cif
_cod_data_source_block           gd
_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 Gd3 N10 O27 Cl3'
_cod_database_code               7706085
_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
 C36, F1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C36, F3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F11, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F16, C26
 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(F9) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(C36)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C36) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F11) \\sim
Ueq, Uanis(F10) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F4)
\\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.001
4.a Riding coordinates:
 O17(H17A,H17B)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C13(H13), C24(H24), C25(H25), C23(H23), C22(H22), C28(H28),
 C48(H48), C43(H43), C53(H53), C33(H33), C38(H38), C80(H80), C66(H66), C68(H68),
  C64(H64), C79(H79), C77(H77), C78(H78), C93(H93), C88(H88), C83(H83)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C19(H19A,H19B,H19C), C17(H17C,H17D,H17E),
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C),
 C57(H57A,H57B,H57C), C75(H75A,H75B,H75C), C74(H74A,H74B,H74C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C), C61(H61A,H61B,H61C), C60(H60A,H60B,H60C), C58(H58A,
 H58B,H58C)
;
_shelx_res_checksum              38793
_shelx_fab_checksum              2633
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'