A mononuclear dysprosium(iii) single-molecule magnet with a non-planar metallacrown
Jiang, Xiao-Feng; Chen, Ming-Guang; Tong, Jia-Ping; Shao, Feng; New Journal of Chemistry 43 (2019) 8704–; doi:10.1039/C9NJ01662G

data_7058359
_publ_section_title
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 A mononuclear dysprosium(iii) single-molecule magnet with a non-planar
 metallacrown
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8704
_journal_paper_doi               10.1039/C9NJ01662G
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C86 H59.4 Dy Ga4 N11 O21, 2(C5 H6 N)'
_chemical_formula_sum            'C96 H71.396 Dy Ga4 N13 O21'
_chemical_formula_weight         2184.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2019-01-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-18 deposited with the CCDC.    2019-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                103.853(7)
_cell_angle_beta                 107.388(8)
_cell_angle_gamma                94.941(7)
_cell_formula_units_Z            2
_cell_length_a                   17.1258(3)
_cell_length_b                   17.3229(3)
_cell_length_c                   18.9600(13)
_cell_measurement_reflns_used    55401
_cell_measurement_temperature    85
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.50
_cell_volume                     5135.6(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      85
_diffrn_measured_fraction_theta_full 0.9785
_diffrn_measured_fraction_theta_max 0.9785
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            79507
_diffrn_reflns_theta_full        68.2325
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    5.599
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.4125
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       prism
_exptl_crystal_F_000             2169.2012
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.4802
_refine_diff_density_min         -2.0649
_refine_diff_density_rms         0.2627
_refine_ls_d_res_high            0.8301
_refine_ls_d_res_low             17.3756
_refine_ls_goodness_of_fit_ref   0.9828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    144
_refine_ls_number_parameters     1219
_refine_ls_number_reflns         18399
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.9828
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.0033
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1790P)^2^+21.0113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2383
_refine_ls_wR_factor_ref         0.2402
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                17779
_reflns_number_total             18399
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9nj01662g2.cif
_cod_data_source_block           DyGa4
_cod_depositor_comments          'Adding full bibliography for 7058359.cif.'
_cod_database_code               7058359
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 H3-H95
 2.1 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 N6(H6), N1(H1), C26(H26), C33(H33), C75(H75), C53(H53), C29(H29), C83(H83),
 C22(H22), C59(H59), C84(H84), C30(H30), C11(H11), C37(H37), C71(H71), C15(H15),
  C86(H86), C17(H17), C31(H31), C52(H52), C9(H9), C44(H44), C18(H18a), C20(H20),
  C68(H68), C48(H48), C64(H64), C50(H50), C70(H70), C74(H74), C76(H76),
 C66(H66), C19(H19), C61(H61), C6(H6a), C7(H7), C4(H4), C62(H62), C28(H28),
 C85(H85), C82(H82), C72(H72), C81(H81), C55(H55), C73(H73), C8(H8), C79(H79),
 C63(H63), C78(H78), C80(H80), C51(H51), C69(H69), C77(H77), C87(H87), C90(H90),
  C95(H95), C91(H91), C40(H40), C42(H42), N12(H12), C89(H89), C39(H39),
 C88(H88), C41(H41), N13(H13), C92(H92), C96(H96), C94(H94), C93(H93), C67(H67)
3.b Idealised tetrahedral OH refined as rotating group:
 O18(H18), O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'