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_1520012
_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 Gd2 Mg2 O22, 2(C6 H16 N), C2 H3 N'
_chemical_formula_sum            'C64 H125 Gd2 Mg2 N3 O22'
_chemical_formula_weight         1651.78
_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                 109.951(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7351(8)
_cell_length_b                   13.1771(6)
_cell_length_c                   21.9189(11)
_cell_measurement_reflns_used    5371
_cell_measurement_temperature    150.1(1)
_cell_measurement_theta_max      27.2300
_cell_measurement_theta_min      3.3720
_cell_volume                     4272.0(4)
_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(1)
_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   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  178.0000 -120.0000 54

  2 omega   42.00   80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673   37.0000   90.0000 38

  3 omega -101.00  -49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.2579 -178.0000  120.0000 52

  4 omega  -51.00   36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.2579   37.0000    0.0000 87
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0103505000
_diffrn_orient_matrix_UB_12      0.0453370000
_diffrn_orient_matrix_UB_13      -0.0135034000
_diffrn_orient_matrix_UB_21      -0.0248097000
_diffrn_orient_matrix_UB_22      -0.0179722000
_diffrn_orient_matrix_UB_23      -0.0316081000
_diffrn_orient_matrix_UB_31      -0.0396810000
_diffrn_orient_matrix_UB_32      0.0228590000
_diffrn_orient_matrix_UB_33      0.0020274000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16558
_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         3.159
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.616
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65549
_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    1.284
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.315
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8731
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0527P)^2^+3.3490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6964
_reflns_number_total             8731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MgGd.cif
_cod_data_source_block           MgGd
_cod_database_code               1520012
_reflns_odcompleteness_completeness 99.74
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-C1L
 1.5 with sigma of 0.02
 C29-C30B
 1.6 with sigma of 0.02
 C31-C29
 1.6 with sigma of 0.02
 C29-C30
 1.6 with sigma of 0.02
 C29-C31B
 1.6 with sigma of 0.02
 C28-C26
 1.6 with sigma of 0.02
 C27-C26
 1.6 with sigma of 0.02
 C26-C1L
 1.6 with sigma of 0.02
 C32-C33
 1.5 with sigma of 0.02
 C32-N2
 1.1 with sigma of 0.02
 C31-C29 \\sim C29-C30
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C3) = Uanis(C3B)
Uanis(C31B) = Uanis(C31) = Uanis(C30B) = Uanis(C30)
Uanis(C4) = Uanis(C4B)
4. Others
 Sof(O11B)=Sof(C1B)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C4B)=Sof(H4BA)=
 Sof(H4BB)=Sof(H4BC)=Sof(H26A)=Sof(H29A)=Sof(C1L)=Sof(H1LA)=Sof(H1LB)=Sof(H1LC)=
 Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31B)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=1-FVAR(1)
 Sof(O11)=Sof(C1)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(H4C)=Sof(H26)=Sof(H29)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C30)=
 Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Fixed Sof: N2(0.5) C32(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5)
5.a Ternary CH refined with riding coordinates:
 C26(H26A), C26(H26), C29(H29), C29(H29A)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.c Idealised Me refined as rotating group:
 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), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C3B(H3BA,
 H3BB,H3BC), C4B(H4BA,H4BB,H4BC), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C1L(H1LA,H1LB,H1LC), C30B(H30D,H30E,
 H30F), C31B(H31D,H31E,H31F), C33(H33A,H33B,H33C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-04-20
_olex2_submission_special_instructions 'No special instructions were received'