Improved single-chain-magnet behavior in a biradical-based nitronyl nitroxide-Cu-Dy chain
Xie, Jing; Li, Hongdao; Yang, Meng; Sun, Juan; Li, Licun; Sutter, Jean-Pascal; Chemical Communications  (2019) –; doi:10.1039/C9CC00570F

data_7123048
_publ_section_title
;
 Improved single-chain-magnet behavior in a biradical-based nitronyl
 nitroxide-Cu-Dy chain
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00570F
_journal_year                    2019
_chemical_formula_moiety         'C60 H38 Cu2 Dy F42 N5 O18'
_chemical_formula_sum            'C60 H38 Cu2 Dy F42 N5 O18'
_chemical_formula_weight         2204.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-19 deposited with the CCDC.    2019-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.45(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.944(4)
_cell_length_b                   20.520(4)
_cell_length_c                   19.008(4)
_cell_measurement_reflns_used    15943
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.8784
_cell_measurement_theta_min      1.3924
_cell_volume                     8132(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0749
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64162
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.816
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8434
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_description       block
_exptl_crystal_F_000             4316
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.899
_refine_diff_density_min         -1.578
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1164
_refine_ls_number_reflns         14313
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1115P)^2^+31.1399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2053
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11334
_reflns_number_total             14313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00570f2.cif
_cod_data_source_block           Dy-Cu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7123048
_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
2. Restrained distances
 H15A-H16C
 2.35 with sigma of 0.01
 H15C-H17A
 2.35 with sigma of 0.01
3. Rigid bond restraints
 C36, C37
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 F14, C36
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 F13, C36
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 F15, C36
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C21 \\sim N4 \\sim C20 \\sim C22 \\sim C23: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C9(H9), C4(H4), C1(H1), C53(H53), C43(H43), C7(H7), C5(H5), C2(H2),
 C33(H33), C58(H58), C38(H38), C48(H48), C28(H28)
5.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C22(H22A,H22B,H22C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C25(H25A,
 H25B,H25C)
;
_shelx_res_checksum              54071
_shelx_hkl_checksum              90847
_olex2_submission_special_instructions 'No special instructions were received'