A new family of heterometallic [Cu<sub>6</sub>M<sub>4</sub>] (M = Gd, Tb, Dy and Y) clusters derived from the combined use of selected pyridyl poly-alcohol ligands.
Anastassiades, Antonis; Alexandropoulos, Dimitris I.; Buch, Christian D.; Piligkos, Stergios; Tasiopoulos, Anastasios J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16202–16211; doi:10.1039/d4dt02054e

data_7717056
_publ_section_title
;
 A new family of heterometallic [Cu<sub>6</sub>M<sub>4</sub>] (M = Gd, Tb,
 Dy and Y) clusters derived from the combined use of selected pyridyl
 poly-alcohol ligands.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16202
_journal_page_last               16211
_journal_paper_doi               10.1039/d4dt02054e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C68 H80 Cu6 N16 O44 Y4, 4(C2 H3 N)'
_chemical_formula_sum            'C76 H92 Cu6 N20 O44 Y4'
_chemical_formula_weight         2726.57
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2kky9d
_audit_creation_date             2024-07-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-15 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.75090(10)
_cell_length_b                   17.75090(10)
_cell_length_c                   16.2759(2)
_cell_measurement_reflns_used    28906
_cell_measurement_temperature    150.1(2)
_cell_measurement_theta_max      79.8550
_cell_measurement_theta_min      2.5140
_cell_volume                     5128.45(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.1(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     48.00 106.00   0.50    1.50    --  111.50 -99.00 -90.00  116
  2  \w     50.00 107.00   0.50    1.50    --  111.50 -79.00 -37.00  114
  3  \w    -18.00  55.00   0.50    0.50    --   49.55 -79.00 -37.00  146
  4  \w    -18.00  21.00   0.50    0.50    --   49.55 -19.00 -30.00   78
  5  \w     65.00 103.00   0.50    1.50    --  111.50   0.00  90.00   76
  6  \w    109.00 176.00   0.50    1.50    --  111.50  38.00  60.00  134
  7  \w    100.00 175.00   0.50    1.50    --  111.50  57.00  30.00  150
  8  \w    115.00 177.00   0.50    1.50    --  111.50  79.00  86.00  124
  9  \w     75.00 119.00   0.50    0.50    --   49.55 126.00   0.00   88
 10  \w     77.00 119.00   0.50    0.50    --   49.55 126.00 -60.00   84
 11  \w     77.00 119.00   0.50    0.50    --   49.55 126.00-150.00   84
 12  \w    -68.00  19.00   0.50    0.50    --  -49.55  79.00  86.00  174
 13  \w    -85.00 -34.00   0.50    1.50    -- -106.00  79.00  86.00  102
 14  \w    -65.00 -34.00   0.50    1.50    -- -106.00  57.00  60.00   62
 15  \w    -62.00 -37.00   0.50    1.50    -- -106.00  57.00  30.00   50
 16  \w    -20.00  19.00   0.50    0.50    --  -49.55  19.00-180.00   78
 17  \w    -62.00 -36.00   0.50    1.50    -- -106.00  57.00-120.00   52
 18  \w    -64.00 -36.00   0.50    1.50    -- -106.00  57.00 -90.00   56
 19  \w   -154.00-107.00   0.50    1.50    -- -106.00   0.00-150.00   94
 20  \w   -141.00-101.00   0.50    1.50    -- -106.00 -38.00-180.00   80
 21  \w   -162.00-129.00   0.50    1.50    -- -106.00 -79.00 -37.00   66
 22  \w   -174.00 -94.00   0.50    1.50    -- -106.00 -57.00   0.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0511480000
_diffrn_orient_matrix_UB_12      -0.0669271000
_diffrn_orient_matrix_UB_13      -0.0228656000
_diffrn_orient_matrix_UB_21      0.0070777000
_diffrn_orient_matrix_UB_22      -0.0308041000
_diffrn_orient_matrix_UB_23      0.0881862000
_diffrn_orient_matrix_UB_31      -0.0698271000
_diffrn_orient_matrix_UB_32      0.0457723000
_diffrn_orient_matrix_UB_33      0.0256601000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35166
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.521
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.060
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.414
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       plate
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.439
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1999 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4579
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0400P)^2^+2.1113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0595
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4544
_reflns_number_total             4579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02054e2.cif
_cod_data_source_block           y4cu6_new
_cod_depositor_comments
'Adding full bibliography for 7717055--7717058.cif.'
_cod_original_cell_volume        5128.45(9)
_cod_database_code               7717056
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C72 H86 Cu6 Y4 N18 O44'
_shelx_estimated_absorpt_t_max   0.616
_shelx_estimated_absorpt_t_min   0.215
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C11-H5
 1.878048 with sigma of 0.02
 Cu2-H5
 3.065512 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C12(H12)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C17(H17), C14(H14), C6(H6), C8(H8), C7(H7), C16(H16), C15(H15)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.721