Dysprosium(III) compounds assembled <i>via</i> a versatile ligand incorporating salicylic hydrazide and 8-hydroxyquinolin units: syntheses, structures and magnetic properties.
Zhang, Li; Montigaud, Vincent; Le Guennic, Boris; Zhang, Peng; Tang, Jinkui; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9457–9466; doi:10.1039/d1dt01525g

data_7707669
_publ_section_title
;
 Dysprosium(III) compounds assembled <i>via</i> a versatile ligand
 incorporating salicylic hydrazide and 8-hydroxyquinolin units: syntheses,
 structures and magnetic properties.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9457
_journal_page_last               9466
_journal_paper_doi               10.1039/d1dt01525g
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C50 H40 Dy2 N6 O12, 3(C H4 O)'
_chemical_formula_sum            'C53 H52 Dy2 N6 O15'
_chemical_formula_weight         1338.00
_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   geom
_audit_creation_date             2021-05-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-06-11 deposited with the CCDC.	2021-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                78.970(2)
_cell_angle_beta                 81.792(2)
_cell_angle_gamma                87.250(2)
_cell_formula_units_Z            1
_cell_length_a                   10.6137(10)
_cell_length_b                   10.8593(10)
_cell_length_c                   11.3970(11)
_cell_measurement_reflns_used    4755
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.48
_cell_volume                     1275.8(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.982
_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  0.0236
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7172
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.195
_diffrn_reflns_theta_min         1.911
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.982
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sadabs; bruker, 2000)'
_exptl_crystal_colour            dark-orange
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.011
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5038
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0434P)^2^+2.6979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4479
_reflns_number_total             5038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01525g2.cif
_cod_data_source_block           2dy2
_cod_depositor_comments
'Adding full bibliography for 7707665--7707669.cif.'
_cod_database_code               7707669
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H6 of O6
 At 1.5 times of:
  All C(H,H,H) groups, H7A of O7, H8A of O8, H3 of O3
2. Restrained distances
 O8-C27
 1.43 with sigma of 0.02
 O7-C26
 1.42 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C27)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O7(0.5) H7A(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 O6(H6), C2(H2), C3(H3A), C4(H4), C7(H7), C8(H8), C10(H10), C13(H13), C14(H14),
  C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
5.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C)
5.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O8(H8A), O7(H7A)
;
_shelx_res_checksum              56808
_shelx_hkl_checksum              38054
_olex2_submission_special_instructions 'No special instructions were received'