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_7055086
_publ_section_title
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 Rhodamine-based field-induced single molecule magnets in Yb(iii) and
 Dy(iii) series
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_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
'C51.2 H38.01 F6 N5 O7 S2 Tb, 2(C H4 O), 0.4(C2 H5)'
_chemical_formula_sum            'C54 H48 F6 N5 O9 S2 Tb'
_chemical_formula_weight         1248.06
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2015-07-27
_audit_creation_method
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Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
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2015-07-29 deposited with the CCDC.
2015-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                118.258(3)
_cell_angle_beta                 97.533(4)
_cell_angle_gamma                91.684(4)
_cell_formula_units_Z            2
_cell_length_a                   13.0712(13)
_cell_length_b                   15.1300(7)
_cell_length_c                   15.7825(7)
_cell_measurement_temperature    296(2)
_cell_volume                     2710.6(3)
_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  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9855
_diffrn_measured_fraction_theta_max 0.9855
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.1048
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24315
_diffrn_reflns_theta_full        24.9988
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.462
_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    1.5290
_exptl_crystal_description       block
_exptl_crystal_F_000             1261.0141
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.1675
_refine_diff_density_min         -2.0278
_refine_diff_density_rms         0.2185
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             13.2536
_refine_ls_goodness_of_fit_ref   1.0612
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    104
_refine_ls_number_parameters     793
_refine_ls_number_reflns         9408
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      1.0450
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.0100
_refine_ls_shift/su_mean         0.0007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+6.1273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1788
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7199
_reflns_number_total             9408
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5nj01724f2.cif
_cod_data_source_block           complex5
_cod_depositor_comments
'Adding full bibliography for 7055083--7055087.cif.'
_cod_database_code               7055086
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H32a,H32b} of C32A, {H37,H37a} of C37, {H38,H38a} of C38,
  {H45,H45a} of C45, {H46,H46a} of C46, {H35a,H35b} of C35, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H32c,H32d} of C32B, All O(H) groups
2. Restrained distances
 C41-C39A \\sim C41-C39B \\sim C49-C47A \\sim C49-C47B
 with sigma of 0.01
 C41-S1A \\sim C41-S1B \\sim C49-S2A \\sim C49-S2B
 with sigma of 0.01
 C40-C39A \\sim C40-C39B \\sim C37-C38 \\sim C48-C47A \\sim C48-C47B \\sim
C45-C46
 with sigma of 0.01
 C40-S1A \\sim C40-S1B \\sim C48-S2A \\sim C48-S2B
 with sigma of 0.01
3. Restrained planarity
 C48, C47B, C46, C45, S2B
 with sigma of 0.01
 C48, C47A, C46, C45, S2A
 with sigma of 0.01
 C40, C39B, C38, C37, S1B
 with sigma of 0.01
 C40, C39A, C38, C37, S1A
 with sigma of 0.01
4. Rigid bond restraints
 C48, S2A, S2B, C47A, C47B, C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 S1A, C40, C39A, S1B, C39B, C37, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C51, C52, F4A, F5A, F6A, F4B, F5B, F6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C28, N5, C32A, C33A, C32B, C33B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C48 \\sim S2A \\sim S2B \\sim C47A \\sim C47B \\sim C45 \\sim C46: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
S1A \\sim C40 \\sim C39A \\sim S1B \\sim C39B \\sim C37 \\sim C38: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C51 \\sim C52 \\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
C28 \\sim N5 \\sim C32A \\sim C33A \\sim C32B \\sim C33B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Sof(H37a)=Sof(H38a)=Sof(C39B)=Sof(H39B)=Sof(S1B)=Sof(H39B)=Sof(H37a)=
 Sof(H38a)=1-FVAR(1)
 Sof(H37)=Sof(H38)=Sof(C39A)=Sof(H39A)=Sof(S1A)=Sof(H39A)=Sof(H37)=Sof(H38)=
 FVAR(1)
 Sof(H45a)=Sof(H46a)=Sof(C47B)=Sof(H47B)=Sof(S2B)=Sof(H47B)=Sof(H45a)=
 Sof(H46a)=1-FVAR(2)
 Sof(H45)=Sof(H46)=Sof(C47A)=Sof(H47A)=Sof(S2A)=Sof(H47A)=Sof(H45)=Sof(H46)=
 FVAR(2)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(3)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(3)
 Sof(H5b)=Sof(C32B)=Sof(H32c)=Sof(H32d)=Sof(C33B)=Sof(H33d)=Sof(H33e)=
 Sof(H33f)=Sof(H5b)=Sof(H32c)=Sof(H32d)=Sof(H33d)=Sof(H33e)=Sof(H33f)=Sof(H5b)=
 Sof(H5b)=Sof(H5b)=Sof(H32c)=Sof(H32d)=Sof(H32d)=1-FVAR(4)
 Sof(H5a)=Sof(C32A)=Sof(H32a)=Sof(H32b)=Sof(C33A)=Sof(H33a)=Sof(H33b)=
 Sof(H33c)=Sof(H5a)=Sof(H32a)=Sof(H32b)=Sof(H33a)=Sof(H33b)=Sof(H33c)=Sof(H5a)=
 Sof(H5a)=FVAR(4)
 Fixed Sof: H28(0)
7.a Secondary CH2 refined with riding coordinates:
 C35(H35a,H35b), C32A(H32a,H32b)
7.b Aromatic/amide H refined with riding coordinates:
 C39B(H39B), C39A(H39A), C47B(H47B), C47A(H47A), C3(H3), C4(H4), C5(H5),
 C16(H16), C15(H15), C14(H14), C13(H13), C24(H24), C20(H20), C30(H30), C27(H27),
  C8(H8), C7(H7), C10(H10), C37(H37), C37(H37a), C38(H38), C38(H38a), C42(H42),
 C45(H45), C45(H45a), C46(H46), C46(H46a), C50(H50), N4(H4a), N5(H5a)
7.c Idealised Me refined as rotating group:
 C1W(H1Wa,H1Wb,H1Wc), C2W(H2Wa,H2Wb,H2Wc), C34(H34a,H34b,H34c), C36(H36a,H36b,
 H36c), C33A(H33a,H33b,H33c), C33B(H33d,H33e,H33f), C22(H22a,H22b,H22c)
7.d Idealised tetrahedral OH refined as rotating group:
 O2W(H2W), O3W(H3W)
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_olex2_submission_special_instructions 'No special instructions were received'