Dinuclear dysprosium SMMs bridged by a neutral bipyrimidine ligand: two crystal systems that depend on different lattice solvents lead to a distinct slow relaxation behaviour.
Sun, Wen-Bin; Yan, Bing; Jia, Li-Hui; Wang, Bing-Wu; Yang, Qian; Cheng, Xin; Li, Hong-Feng; Chen, Peng; Wang, Zhe-Ming; Gao, Song; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8790–8794; doi:10.1039/c6dt01082b

data_7039049
_publ_section_title
;
 Dinuclear dysprosium SMMs bridged by a neutral bipyrimidine ligand: two
 crystal systems that depend on different lattice solvents lead to a
 distinct slow relaxation behaviour.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8790
_journal_page_last               8794
_journal_paper_doi               10.1039/c6dt01082b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C98 H72 Dy2 N4 O12, 2(C H Cl3)'
_chemical_formula_sum            'C100 H74 Cl6 Dy2 N4 O12'
_chemical_formula_weight         2061.33
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2016-04-15 deposited with the CCDC.
2016-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.1311(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8489(3)
_cell_length_b                   19.5533(3)
_cell_length_c                   22.3388(4)
_cell_measurement_reflns_used    29911
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3540
_cell_measurement_theta_min      2.7840
_cell_volume                     9015.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_measured_fraction_theta_max 0.8693
_diffrn_measurement_details
;
  1 omega  -77.00  -13.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -        8.7950    0.0000  -30.0000 64

  2 omega   38.00   88.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -        8.7950    0.0000  -30.0000 50

  3 omega  -24.00   35.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -        8.7950  -38.0000    0.0000 59

  4 omega    0.00   26.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -       -9.6544  -99.0000   90.0000 26

  5 omega   31.00   66.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -       -9.6544   38.0000    0.0000 35

  6 omega  -39.00  -12.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -       -9.6544  -57.0000   60.0000 27

  7 omega  -35.00   10.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -       -9.6544   38.0000    0.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0068261000
_diffrn_orient_matrix_UB_12      -0.0081827000
_diffrn_orient_matrix_UB_13      -0.0311817000
_diffrn_orient_matrix_UB_21      0.0324678000
_diffrn_orient_matrix_UB_22      0.0078217000
_diffrn_orient_matrix_UB_23      -0.0035981000
_diffrn_orient_matrix_UB_31      0.0089812000
_diffrn_orient_matrix_UB_32      -0.0344564000
_diffrn_orient_matrix_UB_33      0.0065896000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            68071
_diffrn_reflns_theta_full        28.52
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.191
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         19915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+12.9034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                15942
_reflns_number_total             19915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01082b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7039049--7039050.cif.'
_cod_original_cell_volume        9015.2(2)
_cod_database_code               7039049
_chemical_oxdiff_formula         'C40 H27 N3 Dy1'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H94 of C94, H95 of C95, H96 of C96, H65 of C65, H64 of C64, H61 of C61, H60
  of C60, H58 of C58, H57 of C57, H56 of C56, H53 of C53, H52 of C52, H51 of
  C51, H50 of C50, H49 of C49, H48 of C48, H67 of C67, H68 of C68, H66 of C66,
  H89 of C89, H88 of C88, H87 of C87, H85 of C85, H83 of C83, H82 of C82, H81
  of C81, H79 of C79, H78 of C78, H77 of C77, H76 of C76, H75 of C75, H74 of
  C74, H73 of C73, H72 of C72, H90 of C90, H91 of C91, H92 of C92, H93 of C93,
  H1 of C1, H2 of C2, H3 of C3, H98 of C98, H102 of C102, H99 of C99, H103 of
  C103, H4 of C4, H7 of C7, H8 of C8, H9 of C9, H10 of C10, H12 of C12, H13 of
  C13, H14 of C14, H15 of C15, H18 of C18, H19 of C19, H21 of C21, H22 of C22,
  H23 of C23, H26 of C26, H27 of C27, H29 of C29, H30 of C30, H35 of C35, H36
  of C36, H38 of C38, H39 of C39, H41 of C41, H42 of C42, H44 of C44, H104 of
  C104, H106 of C106, H110 of C110, H111 of C111
2.a Ternary CH refined with riding coordinates:
 C13(H13), C29(H29)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C14(H14), C15(H15), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C26(H26),
  C27(H27), C30(H30), C35(H35), C36(H36), C38(H38), C39(H39), C41(H41),
 C42(H42), C44(H44), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
  C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C64(H64), C65(H65),
 C66(H66), C67(H67), C68(H68), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76),
  C77(H77), C78(H78), C79(H79), C81(H81), C82(H82), C83(H83), C85(H85),
 C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94),
  C95(H95), C96(H96), C98(H98), C99(H99), C102(H102), C103(H103), C104(H104),
 C106(H106), C110(H110), C111(H111)
;