A family of rare earth complexes with chelating furan biradicals: syntheses, structures and magnetic properties
Tian, Li; Li, Xin; Li, Ting; Liu, Zhong Yi; Wang, Xiuguang; RSC Adv.  (2015) –; doi:10.1039/C5RA13386F

data_7221923
_publ_section_title
;
 A family of rare earth complexes with chelating furan biradicals:
 syntheses, structures and magnetic properties
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA13386F
_journal_year                    2015
_chemical_formula_moiety         '2(C33 H29 F18 N4 O11 Pr)'
_chemical_formula_sum            'C66 H58 F36 N8 O22 Pr2'
_chemical_formula_weight         2281.02
_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
_audit_creation_date             2015-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-07-02 deposited with the CCDC.
2015-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                68.426(3)
_cell_angle_beta                 87.010(3)
_cell_angle_gamma                66.321(3)
_cell_formula_units_Z            2
_cell_length_a                   13.9203(4)
_cell_length_b                   17.1400(5)
_cell_length_c                   21.2848(7)
_cell_measurement_reflns_used    18008
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.5860
_cell_measurement_theta_min      3.7730
_cell_volume                     4297.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -50.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4301   38.0000   30.0000 85

  2 omega  -87.00   41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4301   19.0000 -120.0000 128

  3 omega  -50.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4301   38.0000  -60.0000 85

  4 omega  -51.00   -3.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4301  125.0000   30.0000 48

  5 omega   41.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.4301 -125.0000   30.0000 48

  6 omega   44.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.4301 -125.0000 -150.0000 45

  7 omega   45.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -94.0000   90.0000 61

  8 omega  101.00  167.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  125.0000  150.0000 66

  9 omega   33.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -45.0000   60.0000 43

 10 omega   23.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -94.0000    0.0000 43

 11 omega   43.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000  150.0000 46

 12 omega   31.00   84.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000    0.0000 53

 13 omega  111.00  176.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064   15.0000  -30.0000 65

 14 omega   42.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -45.0000 -120.0000 47

 15 omega   35.00   71.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064 -125.0000 -180.0000 36

 16 omega   29.00  141.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -77.0000  150.0000 112

 17 omega   45.00   78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000  120.0000 33

 18 omega   96.00  122.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064 -125.0000 -180.0000 26

 19 omega   47.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064   15.0000   90.0000 64

 20 omega  148.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064   15.0000   90.0000 29

 21 omega   46.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064   15.0000  -30.0000 52

 22 omega   72.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -94.0000    0.0000 36

 23 omega   65.00  117.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064 -125.0000    0.0000 52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0038443000
_diffrn_orient_matrix_UB_12      -0.0973235000
_diffrn_orient_matrix_UB_13      0.0371377000
_diffrn_orient_matrix_UB_21      -0.0661570000
_diffrn_orient_matrix_UB_22      0.0126370000
_diffrn_orient_matrix_UB_23      -0.0616425000
_diffrn_orient_matrix_UB_31      0.1019690000
_diffrn_orient_matrix_UB_32      -0.0402222000
_diffrn_orient_matrix_UB_33      -0.0309171000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30910
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.489
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.976
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.389
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1296
_refine_ls_number_reflns         15363
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.6938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13809
_reflns_number_total             15363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra13386f2.cif
_cod_data_source_block           a150116a
_cod_database_code               7221923
_audit_block_doi                 10.5517/cc1jbk1g
_chemical_oxdiff_formula         'C H N O Gd'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1'-C3' = C3'-C5' = C6'-C8' = C8'-C10'
 2.51 with sigma of 0.01
 C2-C4 = C7-C9 = C2'-C4' = C7'-C9'
 2.43 with sigma of 0.01
 O4-C9 = O3-C7 = O2-C4 = O1-C2
 1.25 with sigma of 0.01
 C9-C10 = C7-C6 = C5-C4 = C2-C1
 1.54 with sigma of 0.01
 C9-C8 = C8-C7 = C4-C3 = C3-C2
 1.38 with sigma of 0.01
 F12-C10 = F10-C10 = F11-C10 = F8-C6 = F7-C6 = F9-C6 = F6-C5
 1.33 with sigma of 0.01
 F4-C5 = F5-C5 = F2-C1 = F3-C1 = F1-C1
 1.33 with sigma of 0.01
 C10'-F11' = C10'-F12' = C10'-F10'
 1.33 with sigma of 0.01
 F11'-C9' = F10'-C9' = F12'-C9'
 2.43 with sigma of 0.01
 O1'-Pr1 = O2'-Pr1 = O3'-Pr1 = O4'-Pr1
 2.48 with sigma of 0.02
 O1'-C2' = O2'-C4' = O3'-C7' = O4'-C9'
 1.25 with sigma of 0.01
 C1'-C2' = C4'-C5' = C6'-C7' = C9'-C10'
 1.54 with sigma of 0.01
 C1'-F1' = C1'-F2' = C1'-F3' = C5'-F4' = C5'-F5' = C5'-F6'
 1.33 with sigma of 0.01
 C2'-C3' = C3'-C4' = C7'-C8' = C8'-C9'
 1.39 with sigma of 0.01
 F1'-C2' = F2'-C2' = F3'-C2'
 2.37 with sigma of 0.01
 F4'-C4' = F5'-C4' = F6'-C4'
 2.37 with sigma of 0.01
 F7'-C7' = F8'-C7' = F9'-C7'
 2.37 with sigma of 0.01
 F4'-C5' = F5'-C5' = F6'-C5'
 1.33 with sigma of 0.01
 F10'-F11' \\sim F10'-F12' \\sim F11'-F12'
 with sigma of 0.001
 F6-F5 \\sim F5-F4
 with sigma of 0.02
 F5-F4 \\sim F4-F6
 with sigma of 0.02
 F7-F8 \\sim F8-F9
 with sigma of 0.02
 F9-F7 \\sim F7-F8
 with sigma of 0.02
 F4'-F5' \\sim F4'-F6' \\sim F5'-F6'
 with sigma of 0.001
 F10-F12 \\sim F12-F11
 with sigma of 0.02
 F11-F10 \\sim F10-F12
 with sigma of 0.02
 F2-F3 \\sim F3-F1
 with sigma of 0.02
 F3-F1 \\sim F1-F2
 with sigma of 0.02
 F1'-F2' \\sim F1'-F3' \\sim F2'-F3'
 with sigma of 0.001
 F4'-F5' \\sim F4'-F6' \\sim F5'-F6'
 with sigma of 0.001
 F7'-F8' \\sim F7'-F9' \\sim F8'-F9'
 with sigma of 0.001
 F2-C2 \\sim F3-F1
 with sigma of 0.02
 F1-C2 \\sim F2-C2 \\sim F3-C2
 with sigma of 0.002
3. Restrained planarity
 C1', C2', O1', C3', C4', O2', C5'
 with sigma of 0.001
 C6', C7', C8', C9', C10', O4', O3'
 with sigma of 0.001
 C6, C7, C8, C9, C10, O4, O3
 with sigma of 0.01
 C1, C2, O1, C3, C4, O2, C5
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C2') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F3) \\sim Ueq, Uanis(F3') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F9) = Uanis(F6')
Uanis(F8) = Uanis(F4')
Uanis(F7) = Uanis(F5')
Uanis(F6) = Uanis(F8')
Uanis(F4) = Uanis(F7')
Uanis(F5) = Uanis(F9')
Uanis(F6') = Uanis(F9)
Uanis(F5') = Uanis(F8)
Uanis(F4') = Uanis(F7)
Uanis(C10) = Uanis(C10')
Uanis(F11') = Uanis(F11)
Uanis(F10) = Uanis(F10')
Uanis(F12) = Uanis(F12')
Uanis(F3) = Uanis(F3')
Uanis(F2) = Uanis(F2')
Uanis(F1) = Uanis(F1')
Uanis(C9) = Uanis(C9')
Uanis(C8) = Uanis(C8')
Uanis(C7) = Uanis(C4')
Uanis(C6) = Uanis(C5')
Uanis(C5) = Uanis(C6')
Uanis(C4) = Uanis(C7')
Uanis(C3) = Uanis(C3')
Uanis(C2) = Uanis(C2')
Uanis(C1) = Uanis(C1')
Uanis(O4) = Uanis(O4')
Uanis(O3) = Uanis(O2')
Uanis(O2) = Uanis(O3')
Uanis(O1) = Uanis(O1')
5. Others
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(F4')=Sof(F5')=Sof(F6')=Sof(F7')=Sof(F8')=
 Sof(F9')=Sof(F12')=Sof(F10')=Sof(F11')=Sof(O1')=Sof(O2')=Sof(O3')=Sof(O4')=
 Sof(C1')=Sof(C2')=Sof(C3')=Sof(H3')=Sof(C4')=Sof(C5')=Sof(C6')=Sof(C7')=
 Sof(C8')=Sof(H8')=Sof(C9')=Sof(C10')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(C1)=Sof(C2)=
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=
 Sof(C10)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C3'(H3'), C8'(H8'), C13(H13), C24(H24), C25(H25), C36(H36),
 C41(H41), C46(H46), C57(H57), C58(H58)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'