Rhodamine-based field-induced single molecule magnets in Yb(iii) and Dy(iii) series
Huang, Wei; Xu, Jun; Wu, Dayu; Huang, Xingcai; Jiang, Jun; New J. Chem. 39 (2015) 8650–; doi:10.1039/C5NJ01724F

data_7055085
_publ_section_title
;
 Rhodamine-based field-induced single molecule magnets in Yb(iii) and
 Dy(iii) series
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              8650
_journal_paper_doi               10.1039/C5NJ01724F
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C52 H40 Dy F6 N5 O7 S2, C H4 O, 0.5(H2 O)'
_chemical_formula_sum            'C53 H45 Dy F6 N5 O8.5 S2'
_chemical_formula_weight         1228.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-29 deposited with the CCDC.
2015-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                117.175(2)
_cell_angle_beta                 95.878(3)
_cell_angle_gamma                92.955(3)
_cell_formula_units_Z            2
_cell_length_a                   13.001(3)
_cell_length_b                   14.9878(17)
_cell_length_c                   15.6387(19)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.32
_cell_volume                     2680.0(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27582
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.7784
_exptl_absorpt_correction_T_min  0.7072
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.736
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         9269
_refine_ls_number_restraints     1469
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+0.3426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                8111
_reflns_number_total             9269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj01724f2.cif
_cod_data_source_block           complex4
_cod_depositor_comments
'Adding full bibliography for 7055083--7055087.cif.'
_cod_original_formula_sum        'C53 H45 Dy F6 N5 O8.50 S2'
_cod_database_code               7055085
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C49B-C51
 1.35 with sigma of 0.02
 O8-C49
 1.35 with sigma of 0.0001
 C12-S2A \\sim C12-S2B \\sim C4-S1A \\sim C4-S1B
 with sigma of 0.01
 C12-C11A \\sim C12-C11B \\sim C4-C1A \\sim C4-C1B
 with sigma of 0.01
 C5-S1A \\sim C5-S1B \\sim C13-S2A \\sim C13-S2B
 with sigma of 0.01
 C5-C1A \\sim C5-C1B \\sim C13-C11A \\sim C13-C11B
 with sigma of 0.01
3. Restrained planarity
 C4, C1A, C1B, C2, C3, S1A, S1B
 with sigma of 0.01
 C12, C9, C10, S2A, S2B, C11A, C11B
 with sigma of 0.01
4. Rigid bond restraints
 C4, S1A, S1B, C1A, C1B, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C12, S2A, S2B, C11A, C11B, C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C7, C8, F4A, F5A, F6A, F4B, F5B, F6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C52 \\sim C54 \\sim N2: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C1A \\sim C1B \\sim C11A \\sim C11B \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim
C6 \\sim C9 \\sim C10 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C52 \\sim C54 \\sim C7 \\sim C8 \\sim C49A \\sim C49B \\sim C50 \\sim C51 \\sim
C49: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C4 \\sim S1A \\sim S1B \\sim C1A \\sim C1B \\sim C2 \\sim C3: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C12 \\sim S2A \\sim S2B \\sim C11A \\sim C11B \\sim C9 \\sim C10: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C7 \\sim C8 \\sim F4A \\sim F5A \\sim F6A \\sim F4B \\sim F5B \\sim F6B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.001 and sigma for terminal atoms of 0.002
6. Same fragment restrains
{C15, C16, F1, F2, F3} sigma for 1-2: 0.02, 1-3: 0.04
as
{C7, C8, F4A, F5A, F6A}
7. Others
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
 Sof(S1B)=Sof(C1B)=Sof(H1B)=Sof(H2B)=Sof(H3B)=1-FVAR(2)
 Sof(S1A)=Sof(C1A)=Sof(H1A)=Sof(H2A)=Sof(H3A)=FVAR(2)
 Sof(S2B)=Sof(C11B)=Sof(H11B)=Sof(H9B)=Sof(H10A)=1-FVAR(3)
 Sof(S2A)=Sof(C11A)=Sof(H11A)=Sof(H9A)=Sof(H10)=FVAR(3)
 Fixed Sof: H1AA(0.5) H1BB(0.5) C49A(0.5) H49A(0.5) H49B(0.5) C49B(0.5)
 H49C(0.5) H49D(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C51(0.5) H51A(0.5)
 H51B(0.5) H51C(0.5) O9(0.5) H9C(0.5) H9D(0.5)
8.a Free rotating group:
 O9(H9C,H9D)
8.b Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C49A(H49A,H49B), C49B(H49C,H49D)
8.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C11A(H11A), C11B(H11B), C2(H2A), C2(H2B), C3(H3A),
 C3(H3B), C6(H6), C9(H9A), C9(H9B), C10(H10), C10(H10A), C14(H14), C18(H18),
 C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C29(H29), C30(H30), C31(H31),
  C32(H32), C37(H37), C40(H40), C44(H44), C47(H47), N1(H1AA), N1(H1BB), N2(H2)
8.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C54(H54A,H54B,H54C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C49(H49E,H49F,H49G)
8.e Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'