Systematic Study of a Family of Butterfly-Like {M <sub>2</sub> Ln <sub>2</sub> } Molecular Magnets (M = Mg <sup>II</sup> , Mn <sup>III</sup> , Co <sup>II</sup> , Ni <sup>II</sup> , and Cu <sup>II</sup> ; Ln = Y <sup>III</sup> , Gd <sup>III</sup> , Tb <sup>III</sup> , Dy <sup>III</sup> , Ho <sup>III</sup> , and Er <sup>III</sup> )
Moreno Pineda, Eufemio; Chilton, Nicholas F.; Tuna, Floriana; Winpenny, Richard E. P.; McInnes, Eric J. L.; Inorganic Chemistry 54 (2015) 5930–5941; doi:10.1021/acs.inorgchem.5b00746

data_1520011
_publ_section_title
;
 Systematic Study of a Family of Butterfly-Like {M <sub>2</sub> Ln
 <sub>2</sub> } Molecular Magnets (M = Mg <sup>II</sup> , Mn
 <sup>III</sup> , Co <sup>II</sup> , Ni <sup>II</sup> , and Cu
 <sup>II</sup> ; Ln = Y <sup>III</sup> , Gd <sup>III</sup> , Tb
 <sup>III</sup> , Dy <sup>III</sup> , Ho <sup>III</sup> , and Er
 <sup>III</sup> )
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5930
_journal_page_last               5941
_journal_paper_doi               10.1021/acs.inorgchem.5b00746
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C50 H90 Dy2 Mg2 O22, 2(C6 H15 N)'
_chemical_formula_sum            'C62 H120 Dy2 Mg2 N2 O22'
_chemical_formula_weight         1619.21
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.082(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4531(3)
_cell_length_b                   19.5753(4)
_cell_length_c                   14.0907(3)
_cell_measurement_reflns_used    14491
_cell_measurement_temperature    150.1(2)
_cell_measurement_theta_max      28.8360
_cell_measurement_theta_min      3.3920
_cell_volume                     4028.21(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.1(2)
_diffrn_detector_area_resol_mean 16.1428
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   40.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -99.0000   30.0000 26

  2 omega   54.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673 -178.0000 -150.0000 49

  3 omega   35.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -99.0000 -120.0000 31

  4 omega  -64.00   10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -73.0000  -27.0000 74

  5 omega  -83.00  -36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798 -178.0000  -30.0000 47

  6 omega  -67.00  -42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798 -178.0000 -120.0000 25

  7 omega  -53.00   43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   37.0000  -60.0000 96

  8 omega   17.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   77.0000    0.0000 27

  9 omega  -95.00   -1.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -37.0000  120.0000 94
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0306101000
_diffrn_orient_matrix_UB_12      -0.0239681000
_diffrn_orient_matrix_UB_13      -0.0096170000
_diffrn_orient_matrix_UB_21      -0.0374657000
_diffrn_orient_matrix_UB_22      -0.0172718000
_diffrn_orient_matrix_UB_23      -0.0345346000
_diffrn_orient_matrix_UB_31      0.0039117000
_diffrn_orient_matrix_UB_32      0.0210025000
_diffrn_orient_matrix_UB_33      -0.0394099000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32394
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.098
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.365
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         8225
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0259P)^2^+8.2584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7274
_reflns_number_total             8225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MgDy.cif
_cod_data_source_block           MgDy
_cod_original_cell_volume        4028.19(15)
_cod_database_code               1520011
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29-C31
 1.6 with sigma of 0.02
 C29-C30
 1.6 with sigma of 0.02
 C29-C32
 1.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) = Uanis(C32) = Uanis(C30) = Uanis(C27) = Uanis(C28)
Uanis(C29) = Uanis(C26)
Uanis(C28) = Uanis(C26) = Uanis(C27)
4. Others
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(1)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C26(H26)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C),
 C32(H32A,H32B,H32C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-04-20
_olex2_submission_special_instructions 'No special instructions were received'