Slow magnetic relaxation in tris(diphosphanylamido) and tetra(phosphanoamido) dysprosium complexes.
Völcker, Franziska; Lan, Yanhua; Powell, Annie K.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 11471–11475; doi:10.1039/c3dt51078f

data_7021730
_publ_section_title
;
 Slow magnetic relaxation in tris(diphosphanylamido) and
 tetra(phosphanoamido) dysprosium complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11471
_journal_page_last               11475
_journal_paper_doi               10.1039/c3dt51078f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C72 H60 Dy N4 P4, C16 H32 Li O4'
_chemical_formula_sum            'C88 H92 Dy Li N4 O4 P4'
_chemical_formula_weight         1562.98
_chemical_name_systematic
;
?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-15
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.953(3)
_cell_length_b                   24.603(5)
_cell_length_c                   26.133(5)
_cell_measurement_reflns_used    40924
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      1.61
_cell_volume                     9330(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
392 frames, detector distance = 100 mm
;
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1206
_diffrn_reflns_av_unetI/netI     0.3787
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            116665
_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.93
_exptl_absorpt_correction_T_max  0.9068
_exptl_absorpt_correction_T_min  0.7510
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3716
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.046
_platon_squeeze_details
;
;
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.742
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         16986
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.742
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                8300
_reflns_number_total             16986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51078f.txt
_cod_data_source_block           1
_cod_database_code               7021730
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H4 of C4, H5 of C5, H6 of C6, H72 of C72, H29 of C29, H42 of C42, H58 of
C58, {H77A,H77B} of C77, {H79A,H79B} of C79, {H86C,H86D,H86A,H86B} of
C86,
{H78A,H78B} of C78, {H80A,H80B} of C80, {H85A,H85B} of C85,
{H73C,H73D,H73A,
H73B} of C73, {H81C,H81D,H81A,H81B} of C81, {H76A,H76B} of C76B,
{H74A,H74B}
of C74B, {H75A,H75B} of C75B, {H87A,H87B} of C87B, H40 of C40, H41 of
C41,
H44 of C44, H45 of C45, H46 of C46, H47 of C47, H48 of C48, H50 of
C50, H51
of C51, H52 of C52, H53 of C53, H54 of C54, H56 of C56, H57 of C57,
H59 of
C59, H60 of C60, H62B of C62B, H63B of C63B, H64B of C64B, H65B of
C65B, H66B
of C66B, H68 of C68, H69 of C69, H70 of C70, H71 of C71, H9 of C9,
H10 of C10,
H11 of C11, H12 of C12, H18 of C18, H17 of C17, H16 of C16, H15 of
C15, H14
of C14, H20 of C20, H21 of C21, H22 of C22, H23 of C23, H24 of C24,
H26 of
C26, H27 of C27, H28 of C28, H30 of C30, H32 of C32, H33 of C33, H34
of C34,
H35 of C35, H36 of C36, H38 of C38, H39 of C39, {H88A,H88B} of C88B,
{H84A,
H84B} of C84A, {H83A,H83B} of C83A, {H82A,H82B} of C82A, {H75C,H75D}
of C75A,
{H76C,H76D} of C76A, {H84C,H84D} of C84B, {H83C,H83D} of C83B,
{H82C,H82D} of
C82B, {H74C,H74D} of C74A, H62A of C62A, H66A of C66A, H65A of C65A,
H64A of
C64A, H63A of C63A, {H88C,H88D} of C88A, {H87C,H87D} of C87A, H3 of
C3, H2 of
C2, H8 of C8
2. Restrained distances
C87B-C88B
1.48 with sigma of 0.005
O4-C88B
1.44 with sigma of 0.005
3. Others
1-Sof(H76A)=1-Sof(H76A)=1-Sof(H76A)=1-Sof(H76A)=1-Sof(H76A)=1-Sof(H76A) Sof(C75A)=Sof(H75C)=Sof(H75D)=Sof(C76A)=Sof(H76C)=Sof(H76D)
1-Sof(H81D)=1-Sof(H81D)=Sof(H81A)=Sof(H81B)=1-Sof(H81D)=1-Sof(H81D)=1-
Sof(H81D)=1-Sof(H81D)=1-Sof(H81D)=1-Sof(H81D)=1-Sof(H81D)=1-Sof(H81D)=1-
Sof(H81D)=Sof(C84B)=Sof(H84C)=Sof(H84D)=Sof(C83B)=Sof(H83C)=Sof(H83D) Sof(C82B)=Sof(H82C)=Sof(H82D)
1-Sof(H73D)=1-Sof(H73D)=Sof(H73A)=Sof(H73B)=1-Sof(H73D)=1-Sof(H73D)=1-
Sof(H73D)=Sof(C74A)=Sof(H74C)=Sof(H74D)
1-Sof(H86D)=1-Sof(H86D)=Sof(H86A)=Sof(H86B)=1-Sof(H86D)=1-Sof(H86D)=1-

Sof(H86D)=1-Sof(H86D)=1-Sof(H86D)=1-Sof(H86D)=Sof(C88A)=Sof(H88C)=Sof(H88D) Sof(C87A)=Sof(H87C)=Sof(H87D)
Fixed Sof: C62B(0.5) H62B(0.5) C63B(0.5) H63B(0.5) C64B(0.5) H64B(0.5)
C65B(0.5) H65B(0.5) C66B(0.5) H66B(0.5) C62A(0.5) H62A(0.5) C66A(0.5)
H66A(0.5) C65A(0.5) H65A(0.5) C64A(0.5) H64A(0.5) C63A(0.5) H63A(0.5)
4.a Secondary CH2 refined with riding coordinates:
C77(H77A,H77B), C79(H79A,H79B), C86(H86C,H86D), C86(H86A,H86B), C78(H78A,
H78B), C80(H80A,H80B), C85(H85A,H85B), C73(H73C,H73D), C73(H73A,H73B),
C81(H81C,H81D), C81(H81A,H81B), C76B(H76A,H76B), C74B(H74A,H74B),
C75B(H75A,
H75B), C87B(H87A,H87B), C88B(H88A,H88B), C84A(H84A,H84B), C83A(H83A,H83B),
C82A(H82A,H82B), C75A(H75C,H75D), C76A(H76C,H76D), C84B(H84C,H84D),
C83B(H83C,
H83D), C82B(H82C,H82D), C74A(H74C,H74D), C88A(H88C,H88D), C87A(H87C,H87D)
4.b Aromatic/amide H refined with riding coordinates:
C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C8(H8), C9(H9), C10(H10),
C11(H11),
C12(H12), C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C20(H20),
C21(H21),
C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C30(H30),
C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
C40(H40),
C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C59(H59),
C60(H60),
C62B(H62B), C63B(H63B), C64B(H64B), C65B(H65B), C66B(H66B), C68(H68),
C69(H69), C70(H70), C71(H71), C72(H72), C29(H29), C42(H42), C58(H58),
C62A(H62A), C66A(H66A), C65A(H65A), C64A(H64A), C63A(H63A)
;