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_7228761
_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 Gd2 N6 O18'
_chemical_formula_sum            'C68 H50 F36 Gd2 N6 O18'
_chemical_formula_weight         2237.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.07(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.433(3)
_cell_length_b                   17.289(4)
_cell_length_c                   18.334(4)
_cell_measurement_reflns_used    12152
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8625
_cell_measurement_theta_min      1.6200
_cell_volume                     4251.8(17)
_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)
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_computing_structure_solution
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????
;
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 99.9000
_diffrn_measured_fraction_theta_max 27.8625
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -110.0000 - 70.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.0920
              2theta: -19.8860
scan:
    Number of images: 180
               Slice: -110.0000 - 70.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.0920
              2theta: -19.8860
scan:
    Number of images: 180
               Slice: -110.0000 - 70.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.0920
              2theta: -19.8860
;
_diffrn_measurement_device
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Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
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_diffrn_orient_matrix_UB_23      0.0535
_diffrn_orient_matrix_UB_31      -0.0069
_diffrn_orient_matrix_UB_32      0.0517
_diffrn_orient_matrix_UB_33      0.0163
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52795
_diffrn_reflns_theta_full        25.0085
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.692
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.7476
_exptl_crystal_description       block
_exptl_crystal_F_000             2194.3716
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.6346
_refine_diff_density_min         -1.0775
_refine_diff_density_rms         0.1594
_refine_ls_d_res_high            0.8406
_refine_ls_d_res_low             12.5701
_refine_ls_goodness_of_fit_ref   1.0508
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     589
_refine_ls_number_reflns         7492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0508
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1687
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -11
_reflns_number_gt                6801
_reflns_number_total             7492
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7ra06310e2.cif
_cod_data_source_block           Gd
_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_cell_volume        4252.0(15)
_cod_original_formula_sum        'C68 H50 F36 Gd2 N6 O18 '
_cod_database_code               7228761
_diffrn_number_total             10466
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H27 of C27, H26 of C26, H24 of C24, H23 of C23, H3 of C3, H8 of C8, H13 of
  C13, H16 of C16, H17 of C17, H18 of C18, H20 of C20, {H21a,H21b} of C21
 At 1.5 times of:
  {H32a,H32b,H32c} of C32, {H31a,H31b,H31c} of C31, {H29a,H29b,H29c} of C29,
  {H34a,H34b,H34c} of C34
2.a Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C16(H16), C17(H17), C18(H18), C20(H20), C23(H23),
 C24(H24), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C34(H34a,H34b,
 H34c)
;