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_1548187
_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         'C18 H21 Y, C9 H13 P'
_chemical_formula_sum            'C27 H34 P Y'
_chemical_formula_weight         478.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.707(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1790(6)
_cell_length_b                   24.6788(18)
_cell_length_c                   11.5031(10)
_cell_measurement_temperature    100(2)
_cell_volume                     2314.0(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0645
_diffrn_reflns_av_unetI/netI     0.1075
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9217
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.945
_exptl_absorpt_coefficient_mu    2.600
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0574P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3182
_reflns_number_total             4724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms8492-s5.cif
_cod_data_source_block           4
_cod_database_code               1548187
_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. Shared sites
{C5, C5A}
{C4, C4A}
{C3, C3A}
{C2, C2A}
{C1, C1A}
3. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C5A)
Uanis(C4) = Uanis(C4A)
Uanis(C3) = Uanis(C3A)
Uanis(C2) = Uanis(C2A)
Uanis(C1) = Uanis(C1A)
4. Others
 Fixed Sof: C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5)
 C5(0.5) C6(0.5) H6a(0.5) H6b(0.5) H6c(0.5) C1A(0.5) H1A(0.5) C2A(0.5) C3A(0.5)
 H3A(0.5) C4A(0.5) H4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) H6Aa(0.5) H6Ab(0.5)
 H6Ac(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C1A(H1A), C3A(H3A), C4A(H4A), C5A(H5A),
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16),
 C21(H21), C23(H23)
5.b Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C6A(H6Aa,H6Ab,H6Ac), C12(H12a,H12b,H12c), C18(H18a,H18b,
 H18c), C25(H25a,H25b,H25c), C26(H26a,H26b,H26c), C27(H27a,H27b,H27c)
;
_shelx_res_checksum              40904
_shelx_hkl_checksum              10437