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_1520016
_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 Ni2 O22, 2(C6 H16 N)'
_chemical_formula_sum            'C62 H122 Dy2 N2 Ni2 O22'
_chemical_formula_weight         1690.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.5659(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6807(4)
_cell_length_b                   21.2712(4)
_cell_length_c                   18.2888(3)
_cell_measurement_reflns_used    18772
_cell_measurement_temperature    106(1)
_cell_measurement_theta_max      28.6520
_cell_measurement_theta_min      3.1450
_cell_volume                     7881.9(3)
_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 0.999
_diffrn_measurement_details
;
  1 omega  -57.00   70.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.2308   77.0000 -180.0000 254

  2 omega  -55.00   33.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.2308   77.0000   90.0000 176

  3 omega  -13.00  103.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6371   77.0000  -60.0000 232

  4 omega   89.00  118.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6371   77.0000   30.0000 58

  5 omega    2.00   37.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6371   77.0000   30.0000 70
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0302462000
_diffrn_orient_matrix_UB_12      -0.0161597000
_diffrn_orient_matrix_UB_13      0.0016040000
_diffrn_orient_matrix_UB_21      0.0070876000
_diffrn_orient_matrix_UB_22      0.0194845000
_diffrn_orient_matrix_UB_23      -0.0288860000
_diffrn_orient_matrix_UB_31      0.0161043000
_diffrn_orient_matrix_UB_32      0.0217208000
_diffrn_orient_matrix_UB_33      0.0270459000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25520
_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         2.973
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.410
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60526
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+15.4601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7611
_reflns_number_total             8051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NiDy.cif
_cod_data_source_block           NiDy
_cod_database_code               1520016
_reflns_odcompleteness_completeness 99.82
_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.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C30(H30A,H30B), C28(H28A,H28B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C24(H24A,H24B,H24C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C27(H27A,
 H27B,H27C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2012-08-16
_olex2_submission_special_instructions 'No special instructions were received'