Synthesis of a series of hetero-multi-spin Ln<sub>2</sub>Cu<sub>3</sub> complexes based on a methyl-pyrazole nitronyl nitroxide radical with slow magnetic relaxation behaviors.
Shi, Jian Yun; Chen, Peng Yun; Wu, Ming Ze; Tian, Li; Liu, Zhong Yi; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9187–9193; doi:10.1039/c9dt00981g

data_7701673
_publ_section_title
;
 Synthesis of a series of hetero-multi-spin Ln<sub>2</sub>Cu<sub>3</sub>
 complexes based on a methyl-pyrazole nitronyl nitroxide radical with slow
 magnetic relaxation behaviors.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9187
_journal_page_last               9193
_journal_paper_doi               10.1039/c9dt00981g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C52 H40 Cu1.5 Dy F36 N8 O16'
_chemical_formula_sum            'C52 H40 Cu1.5 Dy F36 N8 O16'
_chemical_formula_weight         1974.73
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc21t7vz
_audit_creation_date             2018-09-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-05 deposited with the CCDC.	2019-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                94.322(2)
_cell_angle_beta                 92.4181(17)
_cell_angle_gamma                95.6122(19)
_cell_formula_units_Z            2
_cell_length_a                   11.9061(2)
_cell_length_b                   18.3248(5)
_cell_length_c                   20.3320(5)
_cell_measurement_reflns_used    16578
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.8200
_cell_measurement_theta_min      2.1550
_cell_volume                     4396.66(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00 -30.00   1.00    1.00    --  -41.24 -38.00 120.00   85
  2  \w   -116.00 -18.00   1.00    1.00    --  -41.24 -38.00-150.00   98
  3  \w    -77.00  -2.00   1.00    1.00    --  -41.24 125.00 -60.00   75
  4  \w    -96.00 -65.00   1.00    1.00    --  -41.24-149.00-177.00   31
  5  \w      1.00  35.00   1.00    1.00    --   41.24 -99.00  90.00   34
  6  \w     39.00  97.00   1.00    1.00    --   41.24-125.00-180.00   58
  7  \w    114.00 178.00   1.00    3.91    --  107.08  30.00  90.00   64
  8  \w     80.00 108.00   1.00    3.91    --  107.08  30.00  90.00   28
  9  \w     71.00 133.00   1.00    3.91    --  107.08 -45.00 -90.00   62
 10  \w     45.00 107.00   1.00    3.91    --  107.08 -95.00  60.00   62
 11  \w     60.00 134.00   1.00    3.91    --  107.08 -61.00  90.00   74
 12  \w     38.00 105.00   1.00    3.91    --  107.08 -95.00-120.00   67
 13  \w     89.00 172.00   1.00    3.91    --  107.08  30.00   0.00   83
 14  \w     54.00 103.00   1.00    3.91    --  107.08  15.00 -60.00   49
 15  \w     27.00 109.00   1.00    3.91    --  107.08 -95.00 -30.00   82
 16  \w    151.00 178.00   1.00    3.91    --  107.08  15.00 -60.00   27
 17  \w     86.00 118.00   1.00    3.91    --  107.08-125.00-150.00   32
 18  \w     64.00 118.00   1.00    3.91    --  107.08-125.00 -30.00   54
 19  \w     40.00 114.00   1.00    3.91    --  107.08 -45.00  30.00   74
 20  \w     84.00 128.00   1.00    3.91    --  107.08  45.00-180.00   44
 21  \w     91.00 133.00   1.00    3.91    --  107.08 -45.00 150.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0006740000
_diffrn_orient_matrix_UB_12      -0.0430159000
_diffrn_orient_matrix_UB_13      -0.0681270000
_diffrn_orient_matrix_UB_21      0.0132721000
_diffrn_orient_matrix_UB_22      0.0730107000
_diffrn_orient_matrix_UB_23      -0.0331678000
_diffrn_orient_matrix_UB_31      0.1294975000
_diffrn_orient_matrix_UB_32      0.0009276000
_diffrn_orient_matrix_UB_33      0.0068646000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30784
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         2.182
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.131
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             1939
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
TITL A180926a         P -1         R = 0.09
CELL   11.9061   18.3248   20.3320     94.32     92.42     95.61
SPGR P-1
C101 0.598 0.555 0.126 !       3.99 eA-3
C102 0.624 0.492 0.114 !       3.72 eA-3
C103 0.503 0.481 0.002 !       3.59 eA-3
C104 0.542 0.032 0.483 !       3.09 eA-3
C105 0.514 0.028 0.428 !       2.91 eA-3
C106 0.532 0.461 0.060 !       2.89 eA-3
C107 0.046 1.003 0.110 !       2.82 eA-3
C108 0.953 0.021 0.115 !       2.80 eA-3
C109 0.581 0.095 0.389 !       2.69 eA-3
C110 0.589 0.556 0.051 !       2.60 eA-3
C111 0.142 0.036 0.131 !       2.35 eA-3
C112 0.842 0.990 0.087 !       2.11 eA-3
Q113 0.327 0.637 0.303 !       1.86 eA-3
C114 0.564 0.109 0.326 !       1.85 eA-3
C115 0.764 0.038 0.070 !       1.85 eA-3
Q116 0.198 0.655 0.330 !       1.80 eA-3
C117 0.250 0.022 0.123 !       1.74 eA-3
Q118 0.865 0.802 0.257 !       1.69 eA-3
C119 0.236 0.995 0.156 !       1.67 eA-3
Q120 0.875 0.788 0.228 !       1.60 eA-3
Q121 0.672 0.757 0.096 !       1.55 eA-3
Q122 0.268 0.672 0.370 !       1.52 eA-3
Q123 0.264 0.692 0.304 !       1.43 eA-3
Q124 0.234 0.371 0.339 !       1.42 eA-3
Q125 0.263 0.640 0.249 !       1.41 eA-3
Q126 0.014 0.858 0.291 !       1.31 eA-3
Q127 0.266 0.593 0.394 !       1.27 eA-3
Q128 0.971 0.867 0.302 !       1.21 eA-3
Q129 0.254 0.614 0.308 !       1.17 eA-3
Q130 0.215 0.675 0.222 !       1.10 eA-3
Q131 0.573 0.210 0.156 !       1.09 eA-3
Q132 0.266 0.718 0.228 !       1.06 eA-3
Q133 0.749 0.825 0.111 !       1.06 eA-3
Q134 0.268 0.239 0.121 !       1.03 eA-3
Q135 0.605 0.226 0.062 !       1.02 eA-3
Q136 0.232 0.429 0.425 !       0.99 eA-3
Q137 0.120 0.241 0.144 !       0.97 eA-3
Q138 0.331 0.635 0.404 !       0.96 eA-3
Q139 0.670 0.810 0.408 !       0.95 eA-3
Q140 0.016 0.810 0.198 !       0.95 eA-3
Q141 0.518 0.107 0.127 !       0.90 eA-3
Q142 0.051 0.372 0.374 !       0.86 eA-3
Q143 0.982 0.991 0.424 !       0.86 eA-3
Q144 0.733 0.778 0.421 !       0.86 eA-3
Q145 0.312 0.578 0.297 !       0.86 eA-3
Q146 0.780 0.783 0.488 !       0.79 eA-3
Q147 0.449 0.861 0.211 !       0.79 eA-3
C148 0.455 0.106 0.318 !       0.77 eA-3
C149 0.485 0.118 0.303 !       0.77 eA-3
Q150 0.920 0.583 0.418 !       0.76 eA-3
Q151 0.201 0.233 0.073 !       0.76 eA-3
Q152 0.812 0.258 0.244 !       0.75 eA-3
Q153 1.003 0.056 0.480 !       0.75 eA-3
Q154 0.798 0.186 0.214 !       0.74 eA-3
Q155 0.560 0.139 0.030 !       0.73 eA-3
Q156 0.188 0.607 0.260 !       0.72 eA-3
Q157 0.534 0.829 0.181 !       0.72 eA-3
Q158 0.824 0.824 0.095 !       0.70 eA-3
Q159 0.155 0.717 0.310 !       0.70 eA-3
Q160 0.483 0.621 0.331 !       0.70 eA-3
Q161 0.218 0.727 0.332 !       0.70 eA-3
Q162 0.064 0.980 0.493 !       0.70 eA-3
Q163 0.826 0.275 0.126 !       0.69 eA-3
Q164 0.192 0.180 0.161 !       0.67 eA-3
Q165 0.925 0.035 0.402 !       0.66 eA-3
Q166 0.342 0.704 0.356 !       0.66 eA-3
Q167 0.144 0.249 0.066 !       0.66 eA-3
Q168 0.626 0.390 0.498 !       0.65 eA-3
Q169 0.861 0.314 0.242 !       0.65 eA-3
C170 0.380 0.999 0.164 !       0.65 eA-3
Q171 0.153 0.795 0.203 !       0.65 eA-3
Q172 0.330 0.738 0.268 !       0.64 eA-3
Q173 1.000 0.524 0.218 !       0.64 eA-3
Q174 0.235 0.651 0.125 !       0.64 eA-3
Q175 0.160 0.354 0.355 !       0.64 eA-3
Q176 0.200 0.640 0.375 !       0.63 eA-3
C177 0.668 0.094 0.390 !       0.63 eA-3
Q178 0.206 0.240 0.217 !       0.62 eA-3
Q179 0.376 0.014 0.481 !       0.62 eA-3
Q180 0.363 0.531 0.294 !       0.61 eA-3
Q181 0.249 0.675 0.078 !       0.61 eA-3
Q182 0.392 0.598 0.296 !       0.61 eA-3
Q183 0.346 0.650 0.169 !       0.61 eA-3
Q184 0.281 0.403 0.416 !       0.60 eA-3
Q185 0.983 0.066 0.416 !       0.60 eA-3
Q186 0.422 0.931 0.468 !       0.60 eA-3
C187 0.435 0.959 0.128 !       0.60 eA-3
Q188 0.827 0.570 0.219 !       0.59 eA-3
Q189 0.252 0.620 0.189 !       0.59 eA-3
Q190 0.160 0.567 0.232 !       0.58 eA-3
Q191 0.316 0.567 0.402 !       0.58 eA-3
Q192 0.234 0.516 0.129 !       0.57 eA-3
Q193 0.299 0.642 0.478 !       0.57 eA-3
Q194 0.607 0.867 0.442 !       0.57 eA-3
Q195 0.372 0.552 0.279 !       0.56 eA-3
Q196 0.277 0.195 0.219 !       0.56 eA-3
C197 0.423 0.009 0.129 !       0.56 eA-3
Q198 0.269 0.222 0.226 !       0.56 eA-3
Q199 0.207 0.241 0.011 !       0.56 eA-3
;
_refine_diff_density_max         1.635
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         15698
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1055P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12922
_reflns_number_total             15698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00981g2.cif
_cod_data_source_block           a180926a_sq
_cod_original_cell_volume        4396.67(19)
_cod_original_formula_sum        'C52 H40 Cu1.50 Dy F36 N8 O16'
_cod_database_code               7701673
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(F24) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F26) \\sim Ueq,
Uanis(F25) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F28) \\sim Ueq, Uanis(F30)
\\sim Ueq, Uanis(F29) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F2) \\sim Ueq,
Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F34) \\sim Ueq, Uanis(F36)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C20(H20), C21(H21), C25(H25), C30(H30), C35(H35), C40(H40),
 C45(H45), C50(H50)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C11(H11A,
 H11B,H11C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.193
_oxdiff_exptl_absorpt_empirical_full_min 0.468