Magnetic dynamics of an open-ring tridysprosium complex employing mixed ligands.
Wu, Si-Guo; Peng, Yuan-Yuan; Chen, Yan-Cong; Liu, Jun-Liang; Tong, Ming-Liang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14140–14147; doi:10.1039/d0dt02698k

data_7705452
_publ_section_title
;
 Magnetic dynamics of an open-ring tridysprosium complex employing mixed
 ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14140
_journal_page_last               14147
_journal_paper_doi               10.1039/d0dt02698k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C113 H85 Dy3 N8 O14, 2(Cl O4), C H2 Cl2, 2(C H4 O)'
_chemical_formula_sum            'C116 H95 Cl4 Dy3 N8 O24'
_chemical_formula_weight         2614.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.1480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0092(6)
_cell_length_b                   28.1560(10)
_cell_length_c                   25.5123(9)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.33
_cell_volume                     11675.0(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            107020
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.558
_diffrn_reflns_theta_min         1.846
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.064
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0690 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.8067. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       BAR
_exptl_crystal_F_000             5220
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.154
_refine_diff_density_max         2.908
_refine_diff_density_min         -1.872
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1404
_refine_ls_number_reflns         26789
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+136.5585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18988
_reflns_number_total             26789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02698k2.cif
_cod_data_source_block           Dy3
_cod_depositor_comments          'Adding full bibliography for 7705452.cif.'
_cod_database_code               7705452
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.742
_shelx_estimated_absorpt_t_min   0.575
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C115) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O21) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(C115)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C115) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C113(H11G,H11H)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C0AA(H0AA), C1AA(H1AA), C17(H17), C18(H18), C21(H21), C22(H22),
 C23(H23), C25(H25), C29(H29), C30(H30), C31(H31), C35(H35), C36(H36), C37(H37),
  C40(H40), C42(H42), C43(H43), C44(H44), C47(H47), C047(H047), C48(H48),
 C49(H49), C52(H52), C53(H53), C54(H54), C57(H57), C59(H59), C60(H60), C61(H61),
  C64(H64), C65(H65), C66(H66), C69(H69), C70(H70), C71(H71), C74(H74),
 C76(H76), C77(H77), C78(H78), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85),
  C86(H86), C87(H87), C88(H88), C91(H91), C94(H94), C95(H95), C96(H96),
 C97(H97), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C105(H105),
 C108(H108), C109(H109), C110(H110), C111(H111), C112(H112)
3.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C50(H50A,H50B,H50C), C67(H67A,H67B,
 H67C), C115(H11A,H11B,H11C), C114(H11D,H11E,H11F)
3.d Idealised tetrahedral OH refined as rotating group:
 O15(H15), O16(H16)
;
_shelx_res_checksum              61220
_shelx_fab_checksum              74135
_olex2_submission_special_instructions 'No special instructions were received'