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_1520019
_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 Mn2 O22, 2(C6 H16 N), 3(C2 N)'
_chemical_formula_sum            'C68 H122 Dy2 Mn2 N5 O22'
_chemical_formula_weight         1796.58
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                71.5364(15)
_cell_angle_beta                 64.2521(15)
_cell_angle_gamma                81.4352(15)
_cell_formula_units_Z            1
_cell_length_a                   13.2219(2)
_cell_length_b                   13.5495(3)
_cell_length_c                   14.1560(2)
_cell_measurement_reflns_used    13307
_cell_measurement_temperature    106(1)
_cell_measurement_theta_max      28.6250
_cell_measurement_theta_min      3.2200
_cell_volume                     2166.48(7)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      106(1)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   26.00   58.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6371  -57.0000  -60.0000 64

  2 omega  -23.00   64.50   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6371  -99.0000   90.0000 175

  3 omega   -7.00  113.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6371   57.0000 -150.0000 240

  4 omega  -15.00  115.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6371   77.0000  -60.0000 260

  5 omega  -68.00  -40.50   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6371  -57.0000  -60.0000 55
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0130541000
_diffrn_orient_matrix_UB_12      -0.0067518000
_diffrn_orient_matrix_UB_13      0.0558269000
_diffrn_orient_matrix_UB_21      0.0093136000
_diffrn_orient_matrix_UB_22      0.0536621000
_diffrn_orient_matrix_UB_23      -0.0119515000
_diffrn_orient_matrix_UB_31      -0.0573652000
_diffrn_orient_matrix_UB_32      0.0110101000
_diffrn_orient_matrix_UB_33      0.0102195000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14748
_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         2.962
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.055
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74005
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description
;
;
_exptl_crystal_F_000             923
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8838
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0393P)^2^+2.2910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8482
_reflns_number_total             8838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MnDy.cif
_cod_data_source_block           MnDy
_cod_original_cell_volume        2166.49(7)
_cod_database_code               1520019
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-C34
 1.52 with sigma of 0.02
 N1A-C26A = C26A-C27A
 1.52 with sigma of 0.02
 C26B-C27B
 1.52 with sigma of 0.02
 N1A-C27A
 2.633 with sigma of 0.04
3. Rigid bond restraints
 N3, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N3 \\sim C34 \\sim C35: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(N3) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.01
Uanis(C4A) = Uanis(C3B) = Uanis(C3A) = Uanis(C5B) = Uanis(C5A) = Uanis(C4B)
5. Rigid body (RIGU) restrains
 C27A, C29A, C31A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27B, C29B, C31B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1A, N1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26A, C28A, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26B, C28B, C30B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O2)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=
 Sof(H4BC)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(H5BC)=Sof(N1B)=Sof(H1B)=Sof(C26B)=
 Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28B)=
 Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30B)=
 Sof(H30C)=Sof(H30D)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(N2B)=Sof(C32B)=
 1-FVAR(1)
 Sof(O2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(N1A)=Sof(H1A)=Sof(C26A)=
 Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28A)=
 Sof(H28A)=Sof(H28B)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=
 Sof(H30A)=Sof(H30B)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(N2A)=Sof(C32A)=
 FVAR(1)
 Fixed Sof: N3(0.5) C34(0.5) C35(0.5)
7.a Ternary CH refined with riding coordinates:
 N1A(H1A), N1B(H1B)
7.b Secondary CH2 refined with riding coordinates:
 C26A(H26A,H26B), C28A(H28A,H28B), C30A(H30A,H30B), C26B(H26C,H26D), C28B(H28C,
 H28D), C30B(H30C,H30D)
7.c Idealised Me refined as rotating group:
 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), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC),
 C3B(H3BA,H3BB,H3BC), C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,H5BC), C27A(H27A,H27B,
 H27C), C29A(H29A,H29B,H29C), C31A(H31A,H31B,H31C), C27B(H27D,H27E,H27F),
 C29B(H29D,H29E,H29F), C31B(H31D,H31E,H31F)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2012-09-29
_olex2_submission_special_instructions 'No special instructions were received'