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_7055084
_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 N5 O7 S2 Yb, C H4 O'
_chemical_formula_sum            'C53 H44 F6 N5 O8 S2 Yb'
_chemical_formula_weight         1230.09
_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             2015-07-22
_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                117.719(4)
_cell_angle_beta                 95.949(6)
_cell_angle_gamma                92.878(6)
_cell_formula_units_Z            2
_cell_length_a                   13.003(5)
_cell_length_b                   14.986(2)
_cell_length_c                   15.684(2)
_cell_measurement_temperature    296(2)
_cell_volume                     2674.1(11)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0779
_diffrn_reflns_av_unetI/netI     0.1782
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14856
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.905
_exptl_absorpt_correction_T_max  0.7019
_exptl_absorpt_correction_T_min  0.6372
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1234
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.050
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         9233
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1895
_reflns_number_gt                4843
_reflns_number_total             9233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj01724f2.cif
_cod_data_source_block           complex3
_cod_depositor_comments
'Adding full bibliography for 7055083--7055087.cif.'
_cod_original_cell_volume        2674.0(11)
_cod_database_code               7055084
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C41-C42A = C42A-C43 = C43-C44 = C41-C42B
 1.36 with sigma of 0.02
 C40-S1A \\sim C40-S1B \\sim C49-S2A \\sim C49-S2B
 with sigma of 0.01
 C40-C42A \\sim C40-C42B \\sim C49-C53A \\sim C49-C53B
 with sigma of 0.01
 C41-S1A \\sim C41-S1B \\sim C50-S2A \\sim C50-S2B
 with sigma of 0.01
 C41-C42A \\sim C41-C42B \\sim C50-C53A \\sim C50-C53B
 with sigma of 0.01
3. Restrained planarity
 C41, C42A, C42B, S1A, S1B, C43, C44
 with sigma of 0.01
4. Rigid bond restraints
 S2B, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C41, C42A, S1A, C42B, S1B, C50, C53A, C53B, S2A, S2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C11, C12, C9, C10
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 N1, C2, C1A, C1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C47, C46, F4A, F5A, F6A, F4B, F5B, F6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F2, C37, O7, C49, C8, C12, C12, C13
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C41 \\sim C42A \\sim S1A \\sim C42B \\sim S1B \\sim C50 \\sim C53A \\sim C53B
\\sim S2A \\sim S2B: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N1 \\sim C2 \\sim C1A \\sim C1B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C47 \\sim C46 \\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
Uanis(C27) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
6. Others
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(2)
 Sof(S1B)=Sof(C42B)=Sof(H42B)=Sof(H43A)=Sof(H44A)=1-FVAR(3)
 Sof(S1A)=Sof(C42A)=Sof(H42A)=Sof(H43)=Sof(H44)=FVAR(3)
 Sof(S2B)=Sof(C53B)=Sof(H53B)=Sof(H52A)=Sof(H51A)=1-FVAR(4)
 Sof(S2A)=Sof(C53A)=Sof(H53A)=Sof(H52)=Sof(H51)=FVAR(4)
 Fixed Sof: H2AA(0.5) H2AB(0.5) H2BC(0.5) H2BD(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C2(H2AA,H2AB), C2(H2BC,H2BD)
7.b Aromatic/amide H refined with riding coordinates:
 C42A(H42A), C42B(H42B), C53A(H53A), C53B(H53B), C4(H4), C7(H7), N2(H2),
 C13(H13), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C31(H31),
  C32(H32), C33(H33), C35(H35), C36(H36), C39(H39), C43(H43), C43(H43A),
 C44(H44), C44(H44A), C48(H48), N1(H1), C52(H52), C52(H52A), C51(H51), C51(H51A)
7.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C54(H54A,H54B,
 H54C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC)
7.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'