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_1548184
_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 Dy, C9 H13 P'
_chemical_formula_sum            'C27 H34 Dy P'
_chemical_formula_weight         552.01
_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                 94.741(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1970(5)
_cell_length_b                   24.7447(18)
_cell_length_c                   11.5021(10)
_cell_measurement_reflns_used    5939
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.5090
_cell_measurement_theta_min      3.2540
_cell_volume                     2325.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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      100
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0273370000
_diffrn_orient_matrix_UB_12      -0.0175670000
_diffrn_orient_matrix_UB_13      0.0214147000
_diffrn_orient_matrix_UB_21      -0.0374112000
_diffrn_orient_matrix_UB_22      0.0205777000
_diffrn_orient_matrix_UB_23      -0.0028087000
_diffrn_orient_matrix_UB_31      -0.0304844000
_diffrn_orient_matrix_UB_32      -0.0094540000
_diffrn_orient_matrix_UB_33      -0.0465729000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9055
_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         2.940
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.807
_refine_diff_density_min         -1.831
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4745
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0344P)^2^+5.2157P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3978
_reflns_number_total             4745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms8492-s2.cif
_cod_data_source_block           1
_cod_database_code               1548184
_chemical_oxdiff_formula         Dy1P1C21H50
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
{C6, C6A}
{C12, C12A}
{C9, C9A}
{C8, C8A}
{C15, C15A}
3. Restrained distances
 C8-C27
 1.54 with sigma of 0.02
 C6-C27 \\sim C9-C27
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C12) \\sim
Ueq, Uanis(C15) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C25)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C6) = Uanis(C6A)
Uanis(C12) = Uanis(C12A)
Uanis(C9) = Uanis(C9A)
Uanis(C8) = Uanis(C8A)
Uanis(C15) = Uanis(C15A)
5. Others
 Fixed Sof: C8(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C15A(0.5) H15A(0.5)
 C6(0.5) H6(0.5) C9(0.5) H9(0.5) C12(0.5) H12(0.5) C8A(0.5) H8A(0.5) C15(0.5)
 C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C6A(0.5) H6A(0.5) C9A(0.5) H9A(0.5)
 C12A(0.5) H12A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C15A(H15A), C6(H6), C9(H9), C12(H12), C8A(H8A), C6A(H6A), C9A(H9A),
 C12A(H12A), C16(H16), C1(H1), C4(H4), C11(H11), C19(H19), C20(H20), C22(H22),
 C24(H24)
6.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C28(H28A,H28B,
 H28C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              78905
_shelx_hkl_checksum              99123
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'