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_1548189
_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         'C63 H75 Li P3 Y3, 2(C16 H32 Li O4), C4 H8 O'
_chemical_formula_sum            'C99 H147 Li3 O9 P3 Y3'
_chemical_formula_weight         1861.62
_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                 95.358(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3184(10)
_cell_length_b                   15.7523(10)
_cell_length_c                   27.9702(14)
_cell_measurement_reflns_used    4397
_cell_measurement_temperature    150.01(12)
_cell_measurement_theta_max      23.1650
_cell_measurement_theta_min      3.2980
_cell_volume                     9790.4(9)
_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      150.01(12)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -20.00   26.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.8162  -99.0000    0.0000 46

  2 omega  -84.00    4.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.8162  -57.0000  -60.0000 88

  3 omega   35.00   85.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       23.9100  178.0000  -30.0000 50

  4 omega   21.00  101.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       23.9100   37.0000 -150.0000 80
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0230226000
_diffrn_orient_matrix_UB_12      0.0255735000
_diffrn_orient_matrix_UB_13      -0.0117737000
_diffrn_orient_matrix_UB_21      -0.0035402000
_diffrn_orient_matrix_UB_22      0.0211775000
_diffrn_orient_matrix_UB_23      0.0219354000
_diffrn_orient_matrix_UB_31      0.0218209000
_diffrn_orient_matrix_UB_32      0.0304212000
_diffrn_orient_matrix_UB_33      -0.0053822000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.1384
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            37632
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.256
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88124
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       plate
_exptl_crystal_F_000             3936
_exptl_crystal_preparation       'crystallised from THF'
_exptl_crystal_recrystallization_method 'crystallised from THF'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1275
_refine_ls_number_reflns         17853
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0287P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10127
_reflns_number_total             17853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms8492-s7.cif
_cod_data_source_block           6
_cod_database_code               1548189
_chemical_oxdiff_formula         'Fe1 P4 C48 H40 Cl1'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9A-C98A
 1.42 with sigma of 0.02
 O9A-C95A
 1.42 with sigma of 0.02
 C95A-C96A
 1.54 with sigma of 0.02
 C98A-C97A
 1.54 with sigma of 0.02
 C97A-C96A
 1.39 with sigma of 0.02
 O9A-C96A
 2.346 with sigma of 0.02
 O9A-C97A
 2.346 with sigma of 0.02
 C98A-C96A
 2.335 with sigma of 0.02
 C95A-C97A
 2.335 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C71A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C74A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9A) = Uanis(C95A) = Uanis(C96A) = Uanis(C97A) = Uanis(C98A)
4. Rigid body (RIGU) restrains
 O5A, C91A, C92A, C93A, C94A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6A, C83A, C84A, C85A, C86A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, C87, C88, C89, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7A, C87A, C88A, C89A, C90A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9, C95, C96, C97, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9A, C95A, C96A, C97A, C98A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C83, C84, C85, C86
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C91, C92, C93, C94
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C71, C72, C73, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3A, C71A, C72A, C73A, C74A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O5A)=Sof(C91A)=Sof(H91C)=Sof(H91D)=Sof(C92A)=Sof(H92C)=Sof(H92D)=
 Sof(C93A)=Sof(H93C)=Sof(H93D)=Sof(C94A)=Sof(H94C)=Sof(H94D)=1-FVAR(1)
 Sof(O5)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C93)=
 Sof(H93A)=Sof(H93B)=Sof(C94)=Sof(H94A)=Sof(H94B)=FVAR(1)
 Sof(O6A)=Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(C84A)=Sof(H84C)=Sof(H84D)=
 Sof(C85A)=Sof(H85C)=Sof(H85D)=Sof(C86A)=Sof(H86C)=Sof(H86D)=1-FVAR(2)
 Sof(O6)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C85)=
 Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=FVAR(2)
 Sof(O7A)=Sof(C87A)=Sof(H87C)=Sof(H87D)=Sof(C88A)=Sof(H88C)=Sof(H88D)=
 Sof(C89A)=Sof(H89C)=Sof(H89D)=Sof(C90A)=Sof(H90C)=Sof(H90D)=1-FVAR(3)
 Sof(O7)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(C89)=
 Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=FVAR(3)
 Sof(O9A)=Sof(C95A)=Sof(H95C)=Sof(H95D)=Sof(C96A)=Sof(H96C)=Sof(H96D)=
 Sof(C97A)=Sof(H97C)=Sof(H97D)=Sof(C98A)=Sof(H98C)=Sof(H98D)=1-FVAR(4)
 Sof(O9)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(C97)=
 Sof(H97A)=Sof(H97B)=Sof(C98)=Sof(H98A)=Sof(H98B)=FVAR(4)
 Sof(C71A)=Sof(H71C)=Sof(H71D)=Sof(O3A)=Sof(C74A)=Sof(H74C)=Sof(H74D)=
 Sof(C73A)=Sof(H73C)=Sof(H73D)=Sof(C72A)=Sof(H72C)=Sof(H72D)=1-FVAR(5)
 Sof(O3)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=
 Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,
 H83B), C83A(H83C,H83D), C84(H84A,H84B), C84A(H84C,H84D), C85(H85A,H85B),
 C85A(H85C,H85D), C86(H86A,H86B), C86A(H86C,H86D), C87(H87A,H87B), C87A(H87C,
 H87D), C88(H88A,H88B), C88A(H88C,H88D), C89(H89A,H89B), C89A(H89C,H89D),
 C90(H90A,H90B), C90A(H90C,H90D), C91(H91A,H91B), C91A(H91C,H91D), C92(H92A,
 H92B), C92A(H92C,H92D), C93(H93A,H93B), C93A(H93C,H93D), C94(H94A,H94B),
 C94A(H94C,H94D), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,
 H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B),
  C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C95(H95A,H95B), C95A(H95C,
 H95D), C96(H96A,H96B), C96A(H96C,H96D), C97(H97A,H97B), C97A(H97C,H97D),
 C98(H98A,H98B), C98A(H98C,H98D), C71A(H71C,H71D), C74A(H74C,H74D), C73A(H73C,
 H73D), C72A(H72C,H72D)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34),
 C39(H39), C41(H41), C48(H48), C50(H50), C57(H57), C59(H59)
6.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C18(H18A,H18B,
 H18C), C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C36(H36A,H36B,H36C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C)
;
_shelx_res_checksum              32603
_shelx_hkl_checksum              99273
_olex2_submission_special_instructions 'No special instructions were received'