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_7055087
_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 F6 Ho N5 O7 S2, 2(C H4 O)'
_chemical_formula_sum            'C54 H48 F6 Ho N5 O9 S2'
_chemical_formula_weight         1254.02
_chemical_name_systematic
;
 ? 
;
_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                117.673(4)
_cell_angle_beta                 96.46(2)
_cell_angle_gamma                92.48(2)
_cell_formula_units_Z            2
_cell_length_a                   13.023(4)
_cell_length_b                   15.037(4)
_cell_length_c                   15.687(4)
_cell_measurement_temperature    296(2)
_cell_volume                     2687.3(13)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0330
_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            31041
_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    1.631
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         9359
_refine_ls_number_restraints     416
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+1.2436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                8394
_reflns_number_total             9359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj01724f2.cif
_cod_data_source_block           complex6
_cod_depositor_comments
'Adding full bibliography for 7055083--7055087.cif.'
_cod_database_code               7055087
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H9 of O9, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8
2. Restrained distances
 C4-S1A \\sim C4-S1B \\sim C12-S2A \\sim C12-S2B
 with sigma of 0.01
 C4-C3A \\sim C4-C3B \\sim C1-C2 \\sim C12-C11A \\sim C12-C11B \\sim C9-C10
 with sigma of 0.01
 C5-S1A \\sim C5-S1B \\sim C13-S2A \\sim C13-S2B
 with sigma of 0.01
 C5-C3A \\sim C5-C3B \\sim C13-C11A \\sim C13-C11B
 with sigma of 0.01
3. Restrained planarity
 C1, C2, C3A, C4, S1A
 with sigma of 0.01
 C1, C2, C3B, C4, S1B
 with sigma of 0.01
 C12, C11A, C9, C10, S2A
 with sigma of 0.01
 C12, C11B, C9, C10, S2B
 with sigma of 0.01
4. Rigid bond restraints
 C38, N1, C49A, C53A, C49B, C53B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C7, C8, F1A, F2A, F3A, F1B, F2B, F3B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C48, N2, C66A, C67A, C66B, C67B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C4, S1A, S1B, C3A, C3B, C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C12, C11A, C11B, S2A, S2B, C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C38 \\sim N1 \\sim C49A \\sim C53A \\sim C49B \\sim C53B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C7 \\sim C8 \\sim F1A \\sim F2A \\sim F3A \\sim F1B \\sim F2B \\sim F3B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C48 \\sim N2 \\sim C66A \\sim C67A \\sim C66B \\sim C67B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C4 \\sim S1A \\sim S1B \\sim C3A \\sim C3B \\sim C1 \\sim C2: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C12 \\sim C11A \\sim C11B \\sim S2A \\sim S2B \\sim C9 \\sim C10: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
6. Others
 Sof(H2BB)=Sof(C66B)=Sof(H66C)=Sof(H66D)=Sof(C67B)=Sof(H67D)=Sof(H67E)=
 Sof(H67F)=1-FVAR(1)
 Sof(H2AA)=Sof(C66A)=Sof(H66A)=Sof(H66B)=Sof(C67A)=Sof(H67A)=Sof(H67B)=
 Sof(H67C)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(2)
 Sof(H1BB)=Sof(C49B)=Sof(H49C)=Sof(H49D)=Sof(C53B)=Sof(H53D)=Sof(H53E)=
 Sof(H53F)=1-FVAR(3)
 Sof(H1AA)=Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(C53A)=Sof(H53A)=Sof(H53B)=
 Sof(H53C)=FVAR(3)
 Sof(H1B)=Sof(H2B)=Sof(S1B)=Sof(C3B)=Sof(H3B)=1-FVAR(4)
 Sof(H1A)=Sof(H2A)=Sof(S1A)=Sof(C3A)=Sof(H3A)=FVAR(4)
 Sof(H9B)=Sof(H10A)=Sof(S2B)=Sof(C11B)=Sof(H11B)=1-FVAR(5)
 Sof(H9A)=Sof(H10)=Sof(S2A)=Sof(C11A)=Sof(H11A)=FVAR(5)
7.a Riding coordinates:
 O9(H9)
7.b Secondary CH2 refined with riding coordinates:
 C49A(H49A,H49B), C49B(H49C,H49D), C66A(H66A,H66B), C66B(H66C,H66D)
7.c Me refined with riding coordinates:
 C36(H36A,H36B,H36C), C57(H57A,H57B,H57C), C53A(H53A,H53B,H53C), C53B(H53D,
 H53E,H53F), C47(H47A,H47B,H47C), C67A(H67A,H67B,H67C), C67B(H67D,H67E,H67F)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C6(H6), C9(H9A), C10(H10), C14(H14), C17(H17), C18(H18),
 C19(H19), C23(H23), C24(H24), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32),
  C39(H39), C40(H40), C45(H45), C46(H46), C3A(H3A), C3B(H3B), C11A(H11A),
 C11B(H11B), N1(H1AA), N2(H2AA)
7.e Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C)
7.f Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'