Single-molecule magnets under dc field with an anion effect: self-assembly of pure dysprosium(iii) metallacycles.
Wu, Jianfeng; Yang, Qianqian; Wang, Haoyu; Ge, Yan; Tang, Jinkui; Qi, Zhenhui; Dalton transactions (Cambridge, England : 2003) 50 (2021) 262–269; doi:10.1039/d0dt02869j

data_7705951
_publ_section_title
;
 Single-molecule magnets under dc field with an anion effect:
 self-assembly of pure dysprosium(iii) metallacycles.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              262
_journal_page_last               269
_journal_paper_doi               10.1039/d0dt02869j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C122 H146 Dy6 N48 O16, 12(Br1), 2(C2 H5 O), 8(C H4 O), 9(O)'
_chemical_formula_sum            'C134 H212 Br12 Dy6 N48 O35'
_chemical_formula_weight         4989.42
_chemical_name_systematic        Dy6
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc25fv8r
_audit_creation_date             2020-11-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-09 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.615(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.2137(6)
_cell_length_b                   23.1408(7)
_cell_length_c                   21.4891(5)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    173
_cell_measurement_theta_max      59.91
_cell_measurement_theta_min      2.68
_cell_volume                     9726.5(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.789
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1007
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.789
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63917
_diffrn_reflns_point_group_measured_fraction_full 0.789
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         59.078
_diffrn_reflns_theta_min         2.857
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    15.605
_exptl_absorpt_correction_T_max  0.131
_exptl_absorpt_correction_T_min  0.095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. Rint was 0.2869 before and 0.1007 after correction. The Ratio of minimum to maximum transmission is 0.7252. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       plate
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.152
_refine_diff_density_min         -3.020
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         13874
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0918
_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^)+(0.1181P)^2^+287.0779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2311
_refine_ls_wR_factor_ref         0.2588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9609
_reflns_number_total             13874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02869j2.cif
_cod_data_source_block           Dy6
_cod_depositor_comments
'Adding full bibliography for 7705949--7705952.cif.'
_cod_database_code               7705951
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.203
_shelx_estimated_absorpt_t_min   0.177
_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, All O(H,H) groups
2. Restrained distances
 O11-C64
 1.42 with sigma of 0.02
 O67-C17
 2.6 with sigma of 0.02
 H10-H11
 2.1 with sigma of 0.02
 Br1-C17
 2.7 with sigma of 0.01
 C66-O67
 1.4 with sigma of 0.02
 C66-C17
 1.5 with sigma of 0.02
 H7C-H8A
 2 with sigma of 0.02
 H25-H27B
 1.91 with sigma of 0.02
 Dy1-H3
 3.024589 with sigma of 0.02
 Dy1-H8
 3.022729 with sigma of 0.02
 Dy2-H5
 3.022729 with sigma of 0.02
 Dy3-H6
 2.997409 with sigma of 0.02
3. Rigid bond restraints
 C66, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C64) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O18)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Br6A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O67) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C66) = Uanis(C17)
5. Others
 Sof(Br6A)=1-FVAR(1)
 Sof(Br6)=FVAR(1)
 Sof(Br1A)=1-FVAR(2)
 Sof(Br1)=FVAR(2)
6.a Rotating group:
 O7(H7A,H7B)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B), C21(H21A,H21B), C40(H40A,H40B), C41(H41A,H41B),
 C60(H60A,H60B), C66(H66A,H66B)
6.c Aromatic/amide H refined with riding coordinates:
 O1(H1), O2(H2), O3(H3), O4(H4), O5(H5), O6(H6), O8(H8), C23(H23), C24(H24),
 C25(H25), C36(H36), C38(H38), C43(H43), C44(H44), C45(H45), C5(H5A), C4(H4A),
 C3(H3A), C8(H8A), C13(H13), C18(H18), C67(H67), C16(H16), C33(H33), C48(H48),
 C53(H53), C58(H58), C57(H57), C56(H56)
6.d Fitted pentagon refined as free rotating group:
 N12(C29,C30,N13,C31), C10(C9,N4,C11,N5), C52(N20,C49,C50,N21)
6.e Fitted hexagon refined as free rotating group:
 N9(C22,C23,C24,C25,C26), N16(C35,C36,C37,C38,C39), N17(C42,C43,C44,C45,C46),
 C6(C5,C4,C3,C2,N1), C19(C18,C67,C16,C15,N8), C59(C58,C57,C56,C55,N24)
6.f Tetrahedral OH refined with riding coordinates:
 O11(H11)
6.g Idealised Me refined as rotating group:
 C7(H7C,H7D,H7E), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C27(H27A,H27B,
 H27C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C47(H47A,H47B,H47C), C51(H51A,
 H51B,H51C), C54(H54A,H54B,H54C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C),
 C65(H65A,H65B,H65C), C62(H62A,H62B,H62C), C17(H17A,H17B,H17C), C64(H64A,H64B,
 H64C)
6.h Idealised tetrahedral OH refined as rotating group:
 O10(H10), O12(H12), O9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'