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_1520017
_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 Ni2 O22, 2(C6 H16 N), 2(C2 H3 N)'
_chemical_formula_sum            'C66 H128 Gd2 N4 Ni2 O22'
_chemical_formula_weight         1761.64
_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     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                90
_cell_angle_beta                 111.352(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9042(5)
_cell_length_b                   12.9690(3)
_cell_length_c                   21.7691(6)
_cell_measurement_reflns_used    12107
_cell_measurement_temperature    100.3(1)
_cell_measurement_theta_max      28.5930
_cell_measurement_theta_min      3.1820
_cell_volume                     4181.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      100.3(1)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   25.75   58.00   0.7500    3.5000
omega____ theta____ kappa____ phi______ frames
    -       22.6371  -57.0000  -90.0000 43

  2 omega  -24.00   66.00   0.7500    3.5000
omega____ theta____ kappa____ phi______ frames
    -       22.6371  -99.0000   60.0000 120

  3 omega  -10.00  113.00   0.7500    3.5000
omega____ theta____ kappa____ phi______ frames
    -       22.6371   57.0000 -180.0000 164

  4 omega  -14.00  108.25   0.7500    3.5000
omega____ theta____ kappa____ phi______ frames
    -       22.6371   77.0000  -90.0000 163

  5 omega  -65.00  -39.50   0.7500    3.5000
omega____ theta____ kappa____ phi______ frames
    -       22.6371  -57.0000  -90.0000 34
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0453303000
_diffrn_orient_matrix_UB_12      0.0068409000
_diffrn_orient_matrix_UB_13      -0.0217468000
_diffrn_orient_matrix_UB_21      -0.0154387000
_diffrn_orient_matrix_UB_22      -0.0189695000
_diffrn_orient_matrix_UB_23      0.0245863000
_diffrn_orient_matrix_UB_31      0.0003046000
_diffrn_orient_matrix_UB_32      0.0508483000
_diffrn_orient_matrix_UB_33      0.0120812000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.526
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         8550
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0337P)^2^+11.8749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7655
_reflns_number_total             8550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NIGd.cif
_cod_data_source_block           NiGd
_cod_database_code               1520017
_reflns_odcompleteness_completeness 99.80
_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. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C1P) = Uanis(C4) = Uanis(C3) = Uanis(C1O) = Uanis(C1R) = Uanis(C5)
Uanis(C13) = Uanis(C1A) = Uanis(C15) = Uanis(C1S) = Uanis(C14) = Uanis(C1Q)
3. Rigid body (RIGU) restrains
 N1, H1, C26, H26A, H26B, C27, H27A, H27B, H27C, C28, H28A, H28B, C29, H29A,
 H29B, H29C, C30, H30A, H30B, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1O)=Sof(H1OA)=Sof(H1OB)=Sof(H1OC)=
 Sof(C1P)=Sof(H1PA)=Sof(H1PB)=Sof(H1PC)=Sof(C1Q)=Sof(H1QA)=Sof(H1QB)=Sof(H1QC)=
 Sof(C1R)=Sof(H1RA)=Sof(H1RB)=Sof(H1RC)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=
 1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), 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),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C1A(H1AA,H1AB,
 H1AC), C1O(H1OA,H1OB,H1OC), C1P(H1PA,H1PB,H1PC), C1Q(H1QA,H1QB,H1QC), C1R(H1RA,
 H1RB,H1RC), C1S(H1SA,H1SB,H1SC), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2012-10-23
_olex2_submission_special_instructions 'No special instructions were received'