Syntheses, crystal structures, and magnetic properties of cyclic dimer Ln2L2 complexes constructed from (3-pyridinylmethoxy)phenyl-substituted nitronyl nitroxide ligands
Zhu, Mei; Li, Yang; Jia, Lingjie; Zhang, Li; Zhang, Wei; RSC Adv. 7 (2017) 36895–; doi:10.1039/C7RA06310E

data_7228758
_publ_section_title
;
 Syntheses, crystal structures, and magnetic properties of cyclic dimer
 Ln2L2 complexes constructed from (3-pyridinylmethoxy)phenyl-substituted
 nitronyl nitroxide ligands
;
_journal_issue                   59
_journal_name_full               'RSC Adv.'
_journal_page_first              36895
_journal_paper_doi               10.1039/C7RA06310E
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C68 H50 F36 N6 O18 Tb2'
_chemical_formula_sum            'C68 H50 F36 N6 O18 Tb2'
_chemical_formula_weight         2240.98
_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'
_audit_creation_date             2017-07-04
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_audit_update_record
;
2017-07-06 deposited with the CCDC.
2017-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.48(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.504(3)
_cell_length_b                   17.675(3)
_cell_length_c                   22.376(7)
_cell_measurement_reflns_used    9662
_cell_measurement_temperature    293.1500
_cell_measurement_theta_max      27.8704
_cell_measurement_theta_min      1.5933
_cell_volume                     4403(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      293.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 93.8000
_diffrn_measured_fraction_theta_max 27.8704
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -110.0000 - 70.0000
         Image width: 1.0000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 50.0961
              2theta: -19.8508
scan:
    Number of images: 140
               Slice: -110.0000 - 30.0000
         Image width: 1.0000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 50.0961
              2theta: -19.8508
scan:
    Number of images: 70
               Slice: -110.0000 - -40.0000
         Image width: 1.0000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 50.0961
              2theta: -19.8508
;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0740
_diffrn_orient_matrix_UB_12      -0.0036
_diffrn_orient_matrix_UB_13      -0.0025
_diffrn_orient_matrix_UB_21      0.0013
_diffrn_orient_matrix_UB_22      0.0488
_diffrn_orient_matrix_UB_23      -0.0285
_diffrn_orient_matrix_UB_31      0.0004
_diffrn_orient_matrix_UB_32      0.0272
_diffrn_orient_matrix_UB_33      0.0469
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35120
_diffrn_reflns_theta_full        25.0076
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.60
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.6904
_exptl_crystal_description       Block
_exptl_crystal_F_000             2197.1459
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.9664
_refine_diff_density_min         -1.2043
_refine_diff_density_rms         0.1471
_refine_ls_d_res_high            0.8406
_refine_ls_d_res_low             12.7617
_refine_ls_goodness_of_fit_ref   1.0685
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    45
_refine_ls_number_parameters     575
_refine_ls_number_reflns         7726
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0684
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1925
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -15
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6138
_reflns_number_total             7726
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7ra06310e2.cif
_cod_data_source_block           Tb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_formula_sum        'C68 H50 F36 N6 O18 Tb2 '
_cod_database_code               7228758
_diffrn_number_total             19720
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H16 of C16, H8 of C8, H27 of C27, H23 of C23, H26 of C26, H20 of C20, H18
  of C18, H13 of C13, H24 of C24, {H21a,H21b} of C21, H17 of C17, H3 of C3
 At 1.5 times of:
  {H29a,H29b,H29c} of C29, {H31a,H31b,H31c} of C31, {H32a,H32b,H32c} of C32,
  {H34a,H34b,H34c} of C34
2. Rigid bond restraints
 F7B, C6
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.01
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(F8A) = Uiso(F8B) = Uiso(F7B) = Uiso(F7A) = Uiso(F9B) = Uiso(F9A)
Uiso(F12A) = Uiso(F12B) = Uiso(F10B) = Uiso(F10A) = Uiso(F11A) = Uiso(F11B)
4. Others
 1-Sof(F8B)=1-Sof(F8B)=1-Sof(F8B)=Sof(F7A)=Sof(F8A)=Sof(F9A)
 1-Sof(F11B)=1-Sof(F11B)=1-Sof(F11B)=Sof(F10A)=Sof(F11A)=Sof(F12A)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b)
5.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C27(H27), C23(H23), C26(H26), C20(H20), C18(H18), C13(H13),
 C24(H24), C17(H17), C3(H3), C8(H8)
5.c Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C34(H34a,H34b,H34c), C29(H29a,H29b,
 H29c)
;