Field-induced slow magnetic relaxation in the first Dy(iii)-centered 12-metallacrown-4 double-decker.
Athanasopoulou, Angeliki A.; Baldoví, José J; Carrella, Luca M.; Rentschler, Eva; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15381–15385; doi:10.1039/c9dt02432h

data_7700395
_publ_section_title
;
 Field-induced slow magnetic relaxation in the first Dy(iii)-centered
 12-metallacrown-4 double-decker.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15381
_journal_page_last               15385
_journal_paper_doi               10.1039/c9dt02432h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C56 H36 Dy Ga8 N8 O28, 5(C H4 O), 3(O1), 2(C8 H18 N0.5)'
_chemical_formula_sum            'C77 H92 Dy Ga8 N9 O36'
_chemical_formula_weight         2439.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-15 deposited with the CCDC.    2019-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.093(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6911(4)
_cell_length_b                   18.1247(5)
_cell_length_c                   19.8116(5)
_cell_measurement_reflns_used    55634
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.54
_cell_volume                     4916.2(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
 177 frames, detector distance = 115 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24260
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.886
_diffrn_reflns_theta_min         2.536
_exptl_absorpt_coefficient_mu    2.990
_exptl_absorpt_correction_T_max  0.5866
_exptl_absorpt_correction_T_min  0.3674
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             2438
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.09
_refine_diff_density_max         4.550
_refine_diff_density_min         -1.872
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         10530
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0973
_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^)+(0.1051P)^2^+66.3057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2554
_refine_ls_wR_factor_ref         0.2648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9052
_reflns_number_total             10530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02432h2.cif
_cod_data_source_block           ata245c
_cod_depositor_comments          'Adding full bibliography for 7700395.cif.'
_cod_database_code               7700395
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.396
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H13 of O13, H14 of O14, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H16A of O16, H15 of O15, H18A of O18, H19A of O19
2. Restrained distances
 C53-C54 = C61-C62 = C65-C66
 1.54 with sigma of 0.01
 N5-C51 = C51-C52 = C52-C53 = N5-C59 = C59-C60 = C60-C61 = N5-C63 = C63-C64 =
 C64-C65
 1.52 with sigma of 0.01
 O19-C32
 1.45 with sigma of 0.02
 C31-O18
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C62 \\sim C61 \\sim C60 \\sim C59: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C51 \\sim C52 \\sim C53 \\sim C54: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C32 \\sim O19: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C31 \\sim O18: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O17(0.7) O17A(0.3) O15(0.5) H15(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) N5(0.5) C59(0.5) H59A(0.5) H59B(0.5) C60(0.5) H60A(0.5) H60B(0.5)
 C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5) C63(0.5)
 H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) C65(0.5) H65A(0.5) H65B(0.5)
 C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) O19(0.5) H19A(0.5) O18(0.5) H18A(0.5)
 O20(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 H31C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C59(H59A,H59B), C60(H60A,
 H60B), C61(H61A,H61B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B)
5.b Me refined with riding coordinates:
 C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C)
5.c Aromatic/amide H refined with riding coordinates:
 O13(H13), O14(H14), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10),
 C11(H11), C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26)
5.d Tetrahedral OH refined with riding coordinates:
 O15(H15)
5.e Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C31(H31A,H31B,
 H31C)
5.f Idealised tetrahedral OH refined as rotating group:
 O16(H16A), O19(H19A), O18(H18A)
;
_shelx_res_checksum              81306
_olex2_submission_special_instructions 'No special instructions were received'