Base and Anion Regulated Synthesis of Dysprosium Compounds
Zhong, Fu-Hui; Liu, Chen-Yang; Zheng, Xiao-Yue; Cao, Chen; Peng, Yan; Hu, Zhao-Bo; Liu, Sui-Jun; Wen, He-Rui; CrystEngComm  (2025) –; doi:10.1039/D5CE00940E

data_7251357
_publ_section_title
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 Base and Anion Regulated Synthesis of Dysprosium Compounds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00940E
_journal_year                    2025
_chemical_formula_moiety         'C38 H44 Cl2 Dy2 N8 O4, 2(Cl), 1[]'
_chemical_formula_sum            'C38 H44 Cl4 Dy2 N8 O4'
_chemical_formula_weight         1143.61
_chemical_name_systematic        2
_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_date             2025-05-27
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.11.02 svn.r19aeb66f for OlexSys, GUI svn.r7078)
;
_audit_update_record
;
2025-05-27 deposited with the CCDC.	2025-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                86.868(2)
_cell_angle_beta                 60.809(2)
_cell_angle_gamma                75.300(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1619(7)
_cell_length_b                   11.1679(7)
_cell_length_c                   11.4098(7)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.90
_cell_volume                     1196.98(13)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15097
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.101
_exptl_absorpt_coefficient_mu    3.364
_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    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.647
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4221
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0265
_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^)+2.8634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3903
_reflns_number_total             4221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00940e2.cif
_cod_data_source_block           123_sq
_cod_database_code               7251357
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.824
_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
2. Rigid body (RIGU) restrains
 C18, C17, C16, C15, C14, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N2, C18, C17, C16, C15, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C2, C1, N1, C5, C4, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N2, C14, C15, C16, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C12(H12), C9(H9), C1(H1A), C11(H11),
 C4(H4), C3(H3), C10(H10), C2(H2)
3.c Fitted hexagon refined as free rotating group:
 C14(C15,C16,C17,C18,N2)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              98812
_shelx_fab_checksum              60927
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'