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_7701674
_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 F36 Gd N8 O16'
_chemical_formula_sum            'C52 H40 Cu1.5 F36 Gd N8 O16'
_chemical_formula_weight         1969.48
_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.cc21td09
_audit_creation_date             2018-11-23
_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                94.2310(10)
_cell_angle_beta                 92.598(2)
_cell_angle_gamma                95.684(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9296(3)
_cell_length_b                   18.3338(3)
_cell_length_c                   20.3498(4)
_cell_measurement_reflns_used    34907
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      79.0090
_cell_measurement_theta_min      4.2360
_cell_volume                     4410.63(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -89.00 -59.00   0.50    1.00    --    0.00 -19.00 150.00   60
  2  \w     55.00  86.00   0.50    1.00    --    0.00  77.00  60.00   62
  3  \w    -33.00  34.00   0.50    1.00    --    0.00  77.00  60.00  134
  4  \w     -9.00  25.00   0.50    1.00    --    0.00 -57.00  30.00   68
  5  \w     20.00  88.00   0.50    1.00    --    0.00  77.00  90.00  136
  6  \w     13.00  74.00   0.50    1.00    --    0.00  57.00 150.00  122
  7  \w    -56.00  51.00   0.50    1.00    --    0.00 -19.00 150.00  214
  8  \w     50.00 101.00   0.50    2.00    --  106.20 -77.00-120.00  102
  9  \w     86.00 137.00   0.50    2.00    --  106.20 -82.00  60.00  102
 10  \w     17.00  94.00   0.50    2.00    --  106.20  15.00   0.00  154
 11  \w    130.00 156.00   0.50    2.00    --  106.20  77.00-150.00   52
 12  \w    122.00 196.00   0.50    2.00    --  106.20  82.00 150.00  148
 13  \w     17.00 142.00   0.50    2.00    --  106.20 -82.00 150.00  250
 14  \w     62.00 112.00   0.50    2.00    --  106.20 -82.00 -30.00  100
 15  \w     77.00 107.00   0.50    2.00    --  106.20  77.00-150.00   60
 16  \w     26.00 135.00   0.50    2.00    --  106.20 -45.00-120.00  218
 17  \w     19.00  64.00   0.50    2.00    --  106.20 -82.00  60.00   90
 18  \w     75.00 122.00   0.50    2.00    --  106.20 -77.00  30.00   94
 19  \w     22.00  51.00   0.50    2.00    --  106.20 -77.00  30.00   58
 20  \w    107.00 134.00   0.50    2.00    --  106.20 -45.00  60.00   54
 21  \w     54.00 102.00   0.50    2.00    --  106.20 -82.00-150.00   96
 22  \w     17.00  77.00   0.50    2.00    --  106.20 -30.00-180.00  120
 23  \w     94.00 120.00   0.50    2.00    --  106.20 -30.00-180.00   52
 24  \w     54.00 137.00   0.50    2.00    --  106.20 -82.00 -60.00  166
 25  \w     17.00 140.00   0.50    2.00    --  106.20 -30.00  60.00  246
 26  \w     23.00  48.00   0.50    2.00    --  106.20 -30.00 -30.00   50
 27  \w     69.00 104.00   0.50    2.00    --  106.20 -30.00 -30.00   70
 28  \w     53.00 143.00   0.50    2.00    --  106.20 -82.00  90.00  180
 29  \w     81.00 113.00   0.50    2.00    --  106.20 -82.00   0.00   64
 30  \w     96.00 141.00   0.50    2.00    --  106.20 -82.00-120.00   90
 31  \w     18.00 139.00   0.50    2.00    --  106.20 -30.00 -90.00  242
 32  \w     26.00  97.00   0.50    2.00    --  106.20 -45.00  60.00  142
 33  \w    142.00 169.00   0.50    2.00    --  106.20  45.00 -60.00   54
 34  \w     83.00 108.00   0.50    2.00    --  106.20 -82.00-180.00   50
 35  \w     97.00 196.00   0.50    2.00    --  106.20  15.00   0.00  198
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0180773000
_diffrn_orient_matrix_UB_12      -0.0194729000
_diffrn_orient_matrix_UB_13      0.0718140000
_diffrn_orient_matrix_UB_21      -0.1283345000
_diffrn_orient_matrix_UB_22      -0.0053837000
_diffrn_orient_matrix_UB_23      0.0078096000
_diffrn_orient_matrix_UB_31      -0.0096338000
_diffrn_orient_matrix_UB_32      -0.0822620000
_diffrn_orient_matrix_UB_33      -0.0236739000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1130
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54625
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.135
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       block
_exptl_crystal_F_000             1935
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;
TITL exp_639          P -1         R = 0.10
CELL   11.9296   18.3338   20.3498     94.23     92.60     95.68
SPGR P-1
C101 0.123 0.492 0.111 !       3.70 eA-3
C102 0.097 0.555 0.126 !       3.67 eA-3
C103 0.010 0.485-0.003 !       3.20 eA-3
C104 0.014 0.029 0.426 !       3.11 eA-3
C105 0.034 0.032 0.477 !       3.05 eA-3
C106 0.079 0.093 0.391 !       2.91 eA-3
C107 0.033 0.459 0.063 !       2.87 eA-3
C108 0.451 0.019 0.113 !       2.62 eA-3
C109 0.547 1.001 0.108 !       2.59 eA-3
C110 0.082 0.555 0.049 !       2.50 eA-3
C111 0.654 0.038 0.134 !       2.22 eA-3
C112 0.342 0.988 0.086 !       2.13 eA-3
C113 0.265 0.034 0.072 !       1.74 eA-3
Q114 0.362 0.790 0.281 !       1.64 eA-3
C115 0.766 1.008 0.140 !       1.61 eA-3
Q116 0.735 0.582 0.297 !       1.50 eA-3
Q117 0.784 0.717 0.318 !       1.26 eA-3
Q118 0.735 0.368 0.338 !       1.25 eA-3
Q119 0.794 0.603 0.366 !       1.24 eA-3
Q120 0.825 0.673 0.302 !       1.24 eA-3
Q121 0.514 0.872 0.276 !       1.23 eA-3
Q122 0.186 0.760 0.101 !       1.20 eA-3
Q123 0.737 0.630 0.255 !       1.13 eA-3
Q124 0.103 0.222 0.061 !       1.08 eA-3
Q125 0.725 0.691 0.264 !       1.08 eA-3
Q126 0.707 0.615 0.332 !       1.06 eA-3
Q127 0.826 0.595 0.299 !       1.06 eA-3
Q128 0.456 0.854 0.318 !       1.05 eA-3
Q129 0.746 0.670 0.235 !       1.02 eA-3
C130 0.128 0.987 0.056 !       1.01 eA-3
Q131 0.782 0.694 0.354 !       1.01 eA-3
Q132 0.069 0.194 0.160 !       1.00 eA-3
Q133 0.031 0.120 0.119 !       0.99 eA-3
Q134 0.709 0.696 0.331 !       0.98 eA-3
Q135 0.818 0.622 0.276 !       0.97 eA-3
Q136 0.792 0.665 0.375 !       0.95 eA-3
Q137 0.499 0.796 0.203 !       0.92 eA-3
Q138 0.724 0.426 0.425 !       0.88 eA-3
Q139 0.078 0.255 0.153 !       0.85 eA-3
Q140 0.099 0.265 0.089 !       0.83 eA-3
Q141 0.730 0.513 0.252 !       0.81 eA-3
Q142 0.648 0.643 0.207 !       0.79 eA-3
C143 0.124 0.028 0.479 !       0.78 eA-3
Q144 0.669 0.610 0.403 !       0.78 eA-3
Q145 0.575 0.661 0.308 !       0.76 eA-3
Q146 0.578 0.026 0.502 !       0.75 eA-3
Q147 0.801 0.491 0.325 !       0.75 eA-3
Q148 0.886 0.638 0.413 !       0.75 eA-3
Q149 0.484 0.975 0.439 !       0.74 eA-3
Q150 0.620 0.448 0.436 !       0.74 eA-3
Q151 0.167 0.126 0.360 !       0.73 eA-3
Q152 0.266 0.840 0.104 !       0.71 eA-3
Q153 0.731 0.316 0.161 !       0.71 eA-3
Q154 0.685 0.590 0.160 !       0.71 eA-3
Q155 0.481 0.045 0.450 !       0.70 eA-3
Q156 0.891 0.246 0.141 !       0.70 eA-3
Q157 0.977 0.673 0.376 !       0.70 eA-3
Q158 0.184 0.450 0.080 !       0.69 eA-3
Q159 0.188 0.480 0.149 !       0.67 eA-3
Q160 0.980 0.620 0.330 !       0.66 eA-3
Q161 0.747 0.786 0.438 !       0.65 eA-3
Q162 0.848 0.564 0.251 !       0.64 eA-3
Q163 0.749 0.221 0.105 !       0.64 eA-3
Q164 0.960 0.653 0.313 !       0.63 eA-3
Q165 0.701 0.624 0.117 !       0.63 eA-3
Q166 0.442 0.064 0.499 !       0.62 eA-3
Q167 0.722 0.259 0.223 !       0.62 eA-3
Q168 0.176 0.815 0.418 !       0.61 eA-3
Q169 0.105 0.814 0.363 !       0.61 eA-3
Q170 0.329 0.794 0.460 !       0.61 eA-3
Q171 0.610 0.059 0.199 !       0.60 eA-3
Q172 0.641 0.873 0.424 !       0.60 eA-3
C173 0.927 0.079 0.343 !       0.60 eA-3
Q174 0.345 0.743 0.079 !       0.60 eA-3
Q175 0.753 0.097 0.195 !       0.59 eA-3
Q176 0.654 0.264 0.194 !       0.58 eA-3
Q177 0.876 0.675 0.241 !       0.58 eA-3
Q178 0.644 0.407 0.282 !       0.58 eA-3
Q179 0.347 0.567 0.201 !       0.58 eA-3
Q180 0.534 0.082 0.493 !       0.58 eA-3
Q181 0.734 0.830 0.279 !       0.58 eA-3
Q182 0.387 0.011 0.406 !       0.57 eA-3
Q183 0.702 0.208 0.219 !       0.57 eA-3
Q184 0.715 0.271 0.440 !       0.56 eA-3
Q185 0.496 1.007 0.406 !       0.55 eA-3
Q186 0.719 0.476 0.109 !       0.55 eA-3
Q187 0.860 0.210 0.090 !       0.55 eA-3
Q188 0.033 0.675 0.413 !       0.55 eA-3
Q189 0.684 0.561 0.345 !       0.55 eA-3
Q190 0.886 0.839 0.299 !       0.55 eA-3
Q191 0.689 0.193 0.092 !       0.55 eA-3
Q192 0.048 0.131 0.034 !       0.55 eA-3
Q193 0.873 0.592 0.201 !       0.55 eA-3
Q194 0.409 0.545 0.160 !       0.54 eA-3
Q195 0.969 0.506 0.395 !       0.54 eA-3
Q196 0.707 0.252 0.492 !       0.54 eA-3
Q197 0.206 0.017 0.369 !       0.54 eA-3
Q198 0.746 0.895 0.409 !       0.54 eA-3
Q199 0.715 0.432 0.365 !       0.53 eA-3
;
_refine_diff_density_max         1.339
_refine_diff_density_min         -1.952
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         15689
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0714
_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^)+(0.1578P)^2^+0.3854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14057
_reflns_number_total             15689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00981g2.cif
_cod_data_source_block           exp_639_sq
_cod_original_formula_sum        'C52 H40 Cu1.50 F36 Gd N8 O16'
_cod_database_code               7701674
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.345
_shelx_estimated_absorpt_t_min   0.285
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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(F7) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F29) \\sim
Ueq, Uanis(F30) \\sim Ueq, Uanis(F28) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.005
Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F26) \\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 4.889
_oxdiff_exptl_absorpt_empirical_full_min 0.236