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_1520010
_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 Co2 Gd2 O22, 2(C6 H16 N), C2 N'
_chemical_formula_sum            'C64 H122 Co2 Gd2 N3 O22'
_chemical_formula_weight         1718.00
_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                 110.893(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7469(4)
_cell_length_b                   13.0245(2)
_cell_length_c                   21.9609(5)
_cell_measurement_reflns_used    16359
_cell_measurement_temperature    101.0(3)
_cell_measurement_theta_max      28.0190
_cell_measurement_theta_min      3.1560
_cell_volume                     4207.93(18)
_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      101.0(3)
_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  -20.00   29.20   0.6000   23.2300
omega____ theta____ kappa____ phi______ frames
    -      -25.5278  -99.0000  -30.0000 82

  2 omega  -58.00   72.20   0.6000   23.2300
omega____ theta____ kappa____ phi______ frames
    -       26.7778  -57.0000  150.0000 217

  3 omega  -58.00   72.20   0.6000   23.2300
omega____ theta____ kappa____ phi______ frames
    -       26.7778  -57.0000   30.0000 217

  4 omega  -67.00  -32.80   0.6000   23.2300
omega____ theta____ kappa____ phi______ frames
    -       26.7778  179.0000   90.0000 57

  5 omega  -56.00   70.00   0.6000   23.2300
omega____ theta____ kappa____ phi______ frames
    -       26.7778  -57.0000  -90.0000 210
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0380065000
_diffrn_orient_matrix_UB_12      -0.0321878000
_diffrn_orient_matrix_UB_13      0.0152348000
_diffrn_orient_matrix_UB_21      -0.0236881000
_diffrn_orient_matrix_UB_22      -0.0420495000
_diffrn_orient_matrix_UB_23      -0.0190522000
_diffrn_orient_matrix_UB_31      0.0178211000
_diffrn_orient_matrix_UB_32      0.0126629000
_diffrn_orient_matrix_UB_33      -0.0245108000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28355
_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         3.023
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65164
_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    1.356
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1770
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.551
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         8600
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0474P)^2^+8.8998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7604
_reflns_number_total             8600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CoGd.cif
_cod_data_source_block           CoGd
_cod_original_cell_volume        4207.91(18)
_cod_database_code               1520010
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32-C33
 1.52 with sigma of 0.02
 C31-C29 \\sim C29-C30
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C30A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C4AA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C31A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C32) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C30) = Uanis(C31A) = Uanis(C30A) = Uanis(C31)
Uanis(C2AA) = Uanis(C4)
Uanis(C5AA) = Uanis(C9) = Uanis(C8)
4. Others
 Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(H29A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31D)=
 Sof(H31E)=Sof(H31F)=1-FVAR(2)
 Sof(H29)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(H31C)=FVAR(2)
 Sof(H26A)=Sof(C26A)=Sof(H26B)=Sof(H26C)=Sof(H26D)=1-FVAR(3)
 Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(3)
 Sof(O13)=Sof(C0AA)=1-FVAR(4)
 Sof(O11)=Sof(C1)=FVAR(4)
 Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=
 Sof(H2AC)=1-FVAR(5)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(5)
 Fixed Sof: N1(0.5) C32(0.5) C33(0.5)
5.a Ternary CH refined with riding coordinates:
 C26(H26), C26(H26A), C29(H29), C29(H29A)
5.b Secondary CH2 refined with riding coordinates:
 N11(H11A,H11B)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), 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), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C1AA(H1AA,
 H1AB,H1AC), C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C4AA(H4AA,H4AB,H4AC),
 C5AA(H5AA,H5AB,H5AC), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C26A(H26B,H26C,H26D), C30A(H30D,H30E,H30F),
 C31A(H31D,H31E,H31F)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2012-10-05
_olex2_submission_special_instructions 'No special instructions were received'