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_7717055
_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 Gd4 N16 O44, 3(C2 H3 N)'
_chemical_formula_sum            'C74 H89 Cu6 Gd4 N19 O44'
_chemical_formula_weight         2958.88
_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.cc2kky69
_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                   17.70470(10)
_cell_length_b                   17.70470(10)
_cell_length_c                   16.4257(2)
_cell_measurement_reflns_used    21399
_cell_measurement_temperature    180
_cell_measurement_theta_max      76.0720
_cell_measurement_theta_min      3.5130
_cell_volume                     5148.74(7)
_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      180
_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 0.994
_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    -78.00  10.00   0.40    0.50    --  -47.19  97.00  33.00  220
  2  \w    -18.00  64.00   0.40    0.50    --   47.19 -97.00 -73.00  205
  3  \w   -145.00-117.00   0.40    2.50    -- -106.00 -97.00 -73.00   70
  4  \w   -105.00 -37.00   0.40    2.50    -- -106.00  97.00  33.00  170
  5  \w     87.00 162.20   0.40    2.50    --  106.24  97.00  33.00  188
  6  \w     57.00  98.20   0.40    2.50    --  106.24 -97.00 -73.00  103
  7  \w    -28.00   3.20   0.40    0.50    --  -47.19  19.00 150.00   78
  8  \w     73.00 100.20   0.40    0.50    --   47.19 126.00-120.00   68
  9  \w    -26.00  29.20   0.40    0.50    --   47.19 -19.00-150.00  138
 10  \w     73.00 101.00   0.40    0.50    --   47.19 126.00 -90.00   70
 11  \w    -12.00  29.20   0.40    0.50    --   47.19 -19.00  90.00  103
 12  \w    -92.00 -38.00   0.40    2.50    -- -106.00 126.00 -60.00  135
 13  \w    -67.00 -35.00   0.40    2.50    -- -106.00  61.00-120.00   80
 14  \w   -100.00 -34.00   0.40    2.50    -- -106.00  77.00-120.00  165
 15  \w    -66.00 -36.00   0.40    2.50    -- -106.00  61.00  30.00   75
 16  \w    -68.00 -38.00   0.40    2.50    -- -106.00  61.00-150.00   75
 17  \w     39.00  68.20   0.40    2.50    --  106.24 -61.00   0.00   73
 18  \w     38.00  69.20   0.40    2.50    --  106.24 -61.00 -30.00   78
 19  \w     94.00 170.00   0.40    2.50    --  106.24  15.00-150.00  190
 20  \w     35.00  67.00   0.40    2.50    --  106.24 -61.00 -60.00   80
 21  \w     39.00  67.00   0.40    2.50    --  106.24 -61.00 -90.00   70
 22  \w     42.00  68.00   0.40    2.50    --  106.24 -61.00 120.00   65
 23  \w     41.00  68.20   0.40    2.50    --  106.24 -61.00  60.00   68
 24  \w     38.00  70.00   0.40    2.50    --  106.24 -61.00  90.00   80
;
_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      0.0767119000
_diffrn_orient_matrix_UB_12      -0.0377746000
_diffrn_orient_matrix_UB_13      0.0175120000
_diffrn_orient_matrix_UB_21      -0.0281827000
_diffrn_orient_matrix_UB_22      -0.0231668000
_diffrn_orient_matrix_UB_23      0.0851694000
_diffrn_orient_matrix_UB_31      -0.0299526000
_diffrn_orient_matrix_UB_32      -0.0748397000
_diffrn_orient_matrix_UB_33      -0.0351947000
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35749
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.761
_diffrn_reflns_theta_min         3.530
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.497
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.253
_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    1.909
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 2147 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5354
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0573P)^2^+24.1025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                5158
_reflns_number_total             5354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02054e2.cif
_cod_data_source_block           at_cu6gd4
_cod_depositor_comments
'Adding full bibliography for 7717055--7717058.cif.'
_cod_original_cell_volume        5148.74(9)
_cod_database_code               7717055
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Cu6 Gd4 N8 O40 C100 H100'
_shelx_estimated_absorpt_t_max   0.458
_shelx_estimated_absorpt_t_min   0.088
_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
 C10-H5
 1.880761 with sigma of 0.02
 Cu2-H5
 3.067003 with sigma of 0.02
3. Rigid bond restraints
 O10, N4, O11, O9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N5, C18, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O10 \\sim N4 \\sim O11 \\sim O9: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C19 \\sim C18 \\sim N5: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
5. Others
 Fixed Sof: C18(0.75) N5(0.75) C19(0.75) H19a(0.75) H19b(0.75) H19c(0.75)
6.a Ternary CH refined with riding coordinates:
 C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C11(H11a,H11b), C10(H10a,H10b)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C7(H7), C8(H8), C14(H14), C9(H9), C16(H16), C15(H15)
6.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 1.851
_oxdiff_exptl_absorpt_empirical_full_min 0.619