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_7251358
_publ_section_title
;
 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 H42 Dy2 F6 N8 O10 S2, 2(C F3 O3 S)'
_chemical_formula_sum            'C40 H42 Dy2 F12 N8 O16 S4'
_chemical_formula_weight         1572.05
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-04-07
_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                68.3950(10)
_cell_angle_beta                 83.5880(10)
_cell_angle_gamma                75.9220(10)
_cell_formula_units_Z            1
_cell_length_a                   8.3012(3)
_cell_length_b                   12.6353(5)
_cell_length_c                   14.2845(5)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.93
_cell_volume                     1350.77(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20960
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_min         2.991
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    3.014
_exptl_absorpt_correction_type   none
_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    1.933
_exptl_crystal_description       block
_exptl_crystal_F_000             770
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.926
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.00085(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6197
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+2.3598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5321
_reflns_number_total             6197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00940e2.cif
_cod_data_source_block           a
_cod_database_code               7251358
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.557
_shelx_estimated_absorpt_t_min   0.520
_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,H) groups
2. Restrained distances
 Dy1-H3A \\sim Dy1-H3B
 with sigma of 0.02
3.a Free rotating group:
 O3(H3A,H3B)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C7(H7A,H7B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C18(H18), C12(H12), C2(H2), C17(H17), C15(H15), C4(H4), C9(H9),
 C11(H11), C16(H16), C10(H10), C3(H3)
;
_shelx_res_checksum              63343
_olex2_submission_special_instructions 'No special instructions were received'