Unusual slow magnetic relaxation in a mononuclear copper(ii) complex
Valigura, Dušan; Rajnák, Cyril; Titiš, Ján; Moncoľ, Ján; Bieńko, Alina; Boča, Roman; Dalton Transactions  (2022) –; doi:10.1039/D2DT00023G

data_7709790
_publ_section_title
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 Unusual slow magnetic relaxation in a mononuclear copper(ii) complex
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00023G
_journal_year                    2022
_chemical_formula_moiety         'C21 H17 Cu N5 O15'
_chemical_formula_sum            'C21 H17 Cu N5 O15'
_chemical_formula_weight         642.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-19 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1547(4)
_cell_length_b                   13.7108(3)
_cell_length_c                   8.51570(10)
_cell_measurement_reflns_used    28708
_cell_measurement_temperature    295
_cell_measurement_theta_max      29.4758
_cell_measurement_theta_min      3.0714
_cell_volume                     2469.90(8)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      295.0
_diffrn_detector_area_resol_mean 10.4340
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
  1 omega  -87.00  -33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511  -45.0000  240.0000    0.0000    0.0000 54

  2 omega  -36.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511  -75.0000  120.0000    0.0000    0.0000 58

  3 omega  -89.00  -32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511  -75.0000    0.0000    0.0000    0.0000 57

  4 omega  -36.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511  -45.0000  240.0000    0.0000    0.0000 52

  5 omega  -87.00  -33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511  -45.0000    0.0000    0.0000    0.0000 54

  6 omega  -37.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511  -45.0000    0.0000    0.0000    0.0000 53

  7 omega  -90.00  -32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511  -75.0000  120.0000    0.0000    0.0000 58

  8 omega  -45.00   12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511   72.0000   56.0000    0.0000    0.0000 57

  9 omega  -45.00   13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511   75.0000    0.0000    0.0000    0.0000 58

 10 omega  -39.00   14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511   45.0000  240.0000    0.0000    0.0000 53

 11 phi     92.00  150.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   11.8293    0.0000     -        0.0000    0.0000 58

 12 omega    1.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293   75.0000  120.0000    0.0000    0.0000 36

 13 omega    1.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293 -103.0000   88.0000    0.0000    0.0000 54

 14 omega   34.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293   45.0000  240.0000    0.0000    0.0000 53

 15 omega   -5.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293  -98.0000  342.0000    0.0000    0.0000 57

 16 omega  -62.00  -34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293  -45.0000    0.0000    0.0000    0.0000 28

 17 omega   19.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293 -126.0000  160.0000    0.0000    0.0000 50

 18 omega  -13.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293  -45.0000  240.0000    0.0000    0.0000 53

 19 omega  -11.00   17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293  -45.0000  120.0000    0.0000    0.0000 28

 20 omega   41.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293   45.0000  120.0000    0.0000    0.0000 28

 21 omega   17.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293 -124.0000  134.0000    0.0000    0.0000 52

 22 omega   42.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293 -127.0000  285.0000    0.0000    0.0000 28

 23 omega   11.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293  -45.0000    0.0000    0.0000    0.0000 28

 24 omega   -1.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293 -104.0000  143.0000    0.0000    0.0000 28

 25 omega  -39.00   14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.7511   45.0000  120.0000    0.0000    0.0000 53

 26 omega   19.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293 -126.0000  160.0000    0.0000    0.0000 51

 27 omega   -5.00   53.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.8293  -98.0000  342.0000    0.0000    0.0000 58

 28 phi   -180.00 -118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -11.7511    0.0000     -        0.0000    0.0000 62

 29 phi   -122.00  -59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -11.7511    0.0000     -        0.0000    0.0000 63

 30 phi    -62.00    1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -11.7511    0.0000     -        0.0000    0.0000 63

 31 phi     -2.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -11.7511    0.0000     -        0.0000    0.0000 32
;
_diffrn_measurement_device_type  'Rigaku OD Gemini R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            48688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.592
_diffrn_reflns_theta_min         3.249
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0284 before and 0.0229 after correction.
The Ratio of minimum to maximum transmission is 0.8276.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.5604
_exptl_crystal_size_mid          0.3749
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+1.8844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2554
_reflns_number_total             3303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00023g2.cif
_cod_data_source_block           1_295k
_cod_database_code               7709790
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.611
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: O1W(0.5)
3.a Riding coordinates:
 O1(H1), O1W(H1W)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C9(H9), C11(H11)
;
_shelx_res_checksum              88981
_shelx_hkl_checksum              35289
_olex2_submission_special_instructions 'No special instructions were received'