Structure and assembly mechanism of a centipede-shaped high-nuclear Dy14Cu12 heterometallic nanocluster
Yu, Shui; Hu, Huancheng; Qiu, Zhihui; Zhang, Yuzhen; Liu, Dongcheng; Liang, Yuning; Zou, Hua-Hong; Liang, Fu-Pei; Chen, Zilu; CrystEngComm 25 (2023) 114–121; doi:10.1039/D2CE01291J

data_7246063
_publ_section_title
;
 Structure and assembly mechanism of a centipede-shaped high-nuclear
 Dy14Cu12 heterometallic nanocluster
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              114
_journal_page_last               121
_journal_paper_doi               10.1039/D2CE01291J
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
'C216 H256 Cu12 Dy14 N16 O97, 4(C6H16N), 4(NO3), 2(CH3COO), 6(CH3CN), 5(C2H5OH), 1.5(H2O)'
_chemical_formula_sum            'C266 H377 Cu12 Dy14 N30 O119.5'
_chemical_formula_weight         8944.43
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-11-29 deposited with the CCDC.	2022-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.1080(10)
_cell_angle_beta                 109.6270(10)
_cell_angle_gamma                106.6490(10)
_cell_formula_units_Z            1
_cell_length_a                   18.1682(2)
_cell_length_b                   21.1150(2)
_cell_length_c                   23.7150(3)
_cell_measurement_reflns_used    92099
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      77.7730
_cell_measurement_theta_min      2.7080
_cell_volume                     8161.10(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            126165
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        65.009
_diffrn_reflns_theta_max         65.009
_diffrn_reflns_theta_min         2.711
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.369
_exptl_absorpt_correction_T_max  0.053
_exptl_absorpt_correction_T_min  0.047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       block
_exptl_crystal_F_000             4411
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         2.428
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2094
_refine_ls_number_reflns         27220
_refine_ls_number_restraints     5482
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+36.2182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24503
_reflns_number_total             27220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01291j2.cif
_cod_data_source_block           20201103-CZL-LS-159
_cod_original_formula_sum        'C266 H377 Cu12 Dy14 N30 O119.50'
_cod_database_code               7246063
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.096
_shelx_estimated_absorpt_t_max   0.157
_shelx_res_checksum              7881