Influencing the properties of dysprosium single-molecule magnets with phosphorus donor ligands
Thomas Pugh; Floriana Tuna; Liviu Ungur; David Collison; Eric J.L. McInnes; Liviu F. Chibotaru; Richard A. Layfield; Nature Communications 6 (2015) 7492–; doi:10.1038/ncomms8492

data_1548188
_publ_section_title
;
 Influencing the properties of dysprosium single-molecule magnets with
 phosphorus donor ligands
;
_journal_name_full               'Nature Communications'
_journal_page_first              7492
_journal_paper_doi               10.1038/ncomms8492
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C60 H71.5 P3 Y3, C7 H8, 0.5(C6 H7)'
_chemical_formula_sum            'C70 H83 P3 Y3'
_chemical_formula_weight         1284.00
_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     heavy
_cell_angle_alpha                90
_cell_angle_beta                 91.002(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6328(4)
_cell_length_b                   25.0914(10)
_cell_length_c                   21.5705(7)
_cell_measurement_temperature    150(2)
_cell_volume                     6295.1(4)
_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(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37554
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.730
_exptl_absorpt_coefficient_mu    2.859
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.830
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         12814
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0732P)^2^+12.8808P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1604
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8982
_reflns_number_total             12814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms8492-s6.cif
_cod_data_source_block           5
_cod_database_code               1548188
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C1A, C2A, C2M, C2K, C2J, C2I, C2C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1F, C1E, C1D, C1C, C1B, C1G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1A \\sim C2A \\sim C2M \\sim C2K \\sim C2J \\sim C2I \\sim C2C: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C1D \\sim C1C \\sim C1B \\sim C1F \\sim C1E \\sim C1G: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C1B)
\\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1E) \\sim Ueq,
Uanis(C1F) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C100(0.5) H100(0.5) C101(0.5) H101(0.5) C102(0.5) H102(0.5)
 C103(0.5) H103(0.5) C104(0.5) C105(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C1B(0.5)
 H1B(0.5) C1C(0.5) H1C(0.5) C1D(0.5) H1D(0.5) C1E(0.5) C1F(0.5) H1F(0.5)
 C1G(0.5) H1GA(0.5) H1GB(0.5) H1GC(0.5)
 Fixed U11: C27(0.089835) C1G(0.089937) C1H(0.090462) C6(0.089569)
 C12(0.090479) C1I(0.090136)
 Fixed U22: C27(0.09) C1G(0.09) C1H(0.09) C6(0.09) C12(0.09) C1I(0.09)
 Fixed U33: C27(0.09) C1G(0.09) C1H(0.09) C6(0.09) C12(0.09) C1I(0.09)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
 C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30),
  C31(H31), C36(H36), C38(H38), C43(H43), C44(H44), C45(H45), C46(H46),
 C51(H51), C53(H53), C100(H100), C101(H101), C102(H102), C103(H103), C1A(H1A),
 C2A(H2A), C2I(H2I), C2J(H2J), C2K(H2K), C1B(H1B), C1C(H1C), C1D(H1D), C1F(H1F)
5.b Fitted pentagon refined as free rotating group:
 C100(C101,C102,C103,C104)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C27(H27A,H27B,
 H27C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C105(H10A,H10B,H10C),
 C2C(H2CA,H2CB,H2CC), C1G(H1GA,H1GB,H1GC), C1H(H1HA,H1HB,H1HC), C6(H6A,H6B,H6C),
  C12(H12A,H12B,H12C), C1I(H1IA,H1IB,H1IC)
;