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_1520018
_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 Mn2 O22 Y2, 2(C6 H15 N), 3(C2 N)'
_chemical_formula_sum            'C68 H120 Mn2 N5 O22 Y2'
_chemical_formula_weight         1647.38
_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                71.486(5)
_cell_angle_beta                 64.349(5)
_cell_angle_gamma                81.392(4)
_cell_formula_units_Z            1
_cell_length_a                   13.1987(7)
_cell_length_b                   13.5750(8)
_cell_length_c                   14.1952(7)
_cell_measurement_reflns_used    6092
_cell_measurement_temperature    156(1)
_cell_measurement_theta_max      27.8970
_cell_measurement_theta_min      3.4270
_cell_volume                     2173.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      156(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_details
;
  1 omega   -9.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -99.0000  -60.0000 75

  2 omega  -94.00  -62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000  -30.0000 32

  3 omega  -34.00    3.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -57.0000   60.0000 37

  4 omega  -90.00   11.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000    0.0000 101

  5 omega  -23.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   57.0000   90.0000 72

  6 omega  -43.00  -17.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   57.0000 -150.0000 26

  7 omega  -47.00   48.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   62.0000 -153.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0498256000
_diffrn_orient_matrix_UB_12      0.0290980000
_diffrn_orient_matrix_UB_13      0.0018407000
_diffrn_orient_matrix_UB_21      -0.0281354000
_diffrn_orient_matrix_UB_22      -0.0271833000
_diffrn_orient_matrix_UB_23      0.0558613000
_diffrn_orient_matrix_UB_31      0.0167482000
_diffrn_orient_matrix_UB_32      0.0380957000
_diffrn_orient_matrix_UB_33      0.0147425000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17845
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.859
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.670
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             867
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         9805
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0570P)^2^+1.2660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7813
_reflns_number_total             9805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MnY.cif
_cod_data_source_block           MnY
_cod_original_cell_volume        2173.8(2)
_cod_database_code               1520018
_reflns_odcompleteness_completeness 99.83
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 N1, C26, C27, C28, C29, C30, C31, N1B, C26B, C27B, C28B, C29B, C30B, C31B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C0AA, C3, C4, C5, C3B, C4B, C5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C1A, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C1A, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C32, C33, C32B, C33B, N3, C1A, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(O1B)=Sof(C1B)=Sof(N1B)=Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(C27B)=Sof(H27A)=
 Sof(H27B)=Sof(H27C)=Sof(C28B)=Sof(H28A)=Sof(H28B)=Sof(C29B)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=Sof(C30B)=Sof(H30A)=Sof(H30B)=Sof(C31B)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=Sof(C32B)=Sof(C33B)=1-FVAR(1)
 Sof(O2)=Sof(C1)=Sof(N1)=Sof(C26)=Sof(H26C)=Sof(H26D)=Sof(C27)=Sof(H27D)=
 Sof(H27E)=Sof(H27F)=Sof(C28)=Sof(H28C)=Sof(H28D)=Sof(C29)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30)=Sof(H30C)=Sof(H30D)=Sof(C31)=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 Sof(C32)=Sof(C33)=FVAR(1)
 Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=
 Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(H5BC)=1-FVAR(2)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(2)
 Fixed Sof: N3(0.5) C1A(0.5) C2(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26C,H26D), C28(H28C,H28D), C30(H30C,H30D), C26B(H26A,H26B), C28B(H28A,
 H28B), C30B(H30A,H30B)
4.b 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), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3B(H3BA,H3BB,
 H3BC), C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,H5BC), C27(H27D,H27E,H27F), C29(H29D,
 H29E,H29F), C31(H31D,H31E,H31F), C27B(H27A,H27B,H27C), C29B(H29A,H29B,H29C),
 C31B(H31A,H31B,H31C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-06-08
_olex2_submission_special_instructions 'No special instructions were received'