Probing the magnetic relaxation and magnetic moment arrangement in a series of Dy4 squares.
Wu, Jianfeng; Lin, Shuang-Yan; Shen, Si; Li, Xiao-Lei; Zhao, Lang; Zhang, Li; Tang, Jinkui; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1577–1584; doi:10.1039/c6dt04456e

data_7041580
_publ_section_title
;
 Probing the magnetic relaxation and magnetic moment arrangement in a
 series of Dy4 squares.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1577
_journal_page_last               1584
_journal_paper_doi               10.1039/c6dt04456e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C48 H60 Dy4 N4 O21, C H3 O, 1.5(N O3), 1.5(O)'
_chemical_formula_sum            'C49 H74.5 Dy4 N5.5 O28'
_chemical_formula_weight         1838.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/cc1k2khp
_audit_creation_date             2016-12-18
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5273)
;
_audit_update_record
;
2016-12-18 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.2230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.3361(9)
_cell_length_b                   26.2199(9)
_cell_length_c                   22.9128(8)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.35
_cell_volume                     16410.4(10)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0501
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45670
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    3.667
_exptl_absorpt_correction_T_max  0.463
_exptl_absorpt_correction_T_min  0.447
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             7160
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.299
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         16128
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0672P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10609
_reflns_number_total             16128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04456e2.cif
_cod_data_source_block           s
_cod_depositor_comments
'Adding full bibliography for 7041578--7041580.cif.'
_cod_original_formula_sum        'C49 H74.50 Dy4 N5.50 O28'
_cod_database_code               7041580
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C49-O25
 1.43 with sigma of 0.02
 C35-H13 = C11-H4A = C23-H9 = C48-H16A
 1.99 with sigma of 0.02
 O13-H13 = O4-H4A = O9-H9 = O16-H16A
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24) \\sim Ueq,
Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O29)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C23(H23A,H23B), C24(H24A,H24B), C35(H35A,
 H35B), C36(H36A,H36B), C47(H47A,H47B), C48(H48A,H48B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C15(H15), C16(H16), C17(H17), C20(H20),
 C27(H27), C28(H28), C29(H29), C32(H32), C39(H39), C40(H40), C41(H41), C44(H44)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C22(H22A,H22B,
 H22C), C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C46(H46A,
 H46B,H46C), C49(H49A,H49B,H49C)
4.d Idealised tetrahedral OH refined as rotating group:
 O4(H4A), O9(H9), O13(H13), O16(H16A)
;
_olex2_submission_special_instructions 'No special instructions were received'