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_7221922
_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         'C33 H29 Ce F18 N4 O11'
_chemical_formula_sum            'C33 H29 Ce F18 N4 O11'
_chemical_formula_weight         1139.72
_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                108.562(3)
_cell_angle_beta                 93.305(2)
_cell_angle_gamma                113.769(3)
_cell_formula_units_Z            4
_cell_length_a                   14.1078(4)
_cell_length_b                   17.1982(6)
_cell_length_c                   21.4263(5)
_cell_measurement_reflns_used    12451
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.6010
_cell_measurement_theta_min      3.4540
_cell_volume                     4405.4(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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    4.00   31.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -40.4301   38.0000   60.0000 27

  2 omega  -44.00   31.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -40.4301   38.0000  150.0000 75

  3 omega  -49.00   34.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -40.4301   38.0000   30.0000 83

  4 omega    8.00   33.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -       40.4301   77.0000 -120.0000 25

  5 omega   77.00  174.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064   30.0000 -150.0000 97

  6 omega   81.00  108.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -94.0000    0.0000 27

  7 omega   53.00   90.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000   60.0000 37

  8 omega   55.00   96.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -45.0000  120.0000 41

  9 omega   89.00  178.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064   30.0000  120.0000 89

 10 omega   48.00   84.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000 -120.0000 36

 11 omega   41.00  105.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -94.0000  -60.0000 64

 12 omega   95.00  122.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064 -125.0000 -150.0000 27

 13 omega   44.00   97.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -94.0000 -120.0000 53

 14 omega   46.00  141.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -77.0000    0.0000 95

 15 omega   42.00   78.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -       40.4301  -99.0000  120.0000 36

 16 omega   35.00   76.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -       40.4301  -99.0000   30.0000 41

 17 omega   30.00   89.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000  -60.0000 59

 18 omega   35.00   79.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000 -150.0000 44

 19 omega   30.00   77.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000 -180.0000 47

 20 omega   31.00   75.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000    0.0000 44

 21 omega   33.00   60.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -94.0000    0.0000 27

 22 omega   48.00  104.00   1.0000   38.9800
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -94.0000  150.0000 56

 23 omega    5.00   32.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -40.4301   38.0000 -180.0000 27

 24 omega -114.00  -11.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -40.4301  -57.0000 -120.0000 103
;
_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      -0.0435965000
_diffrn_orient_matrix_UB_12      -0.1038092000
_diffrn_orient_matrix_UB_13      -0.0393534000
_diffrn_orient_matrix_UB_21      -0.1012846000
_diffrn_orient_matrix_UB_22      -0.0166870000
_diffrn_orient_matrix_UB_23      0.0283420000
_diffrn_orient_matrix_UB_31      -0.0525700000
_diffrn_orient_matrix_UB_32      0.0090507000
_diffrn_orient_matrix_UB_33      -0.0606426000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29735
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.074
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         3.464
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31103
_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    1.718
_exptl_crystal_description       block
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.150
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1223
_refine_ls_number_reflns         15707
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0741
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+24.8531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10986
_reflns_number_total             15707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra13386f2.cif
_cod_data_source_block           a150306c
_cod_original_cell_volume        4405.4(2)
_cod_database_code               7221922
_audit_block_doi                 10.5517/cc1jbjn1
_chemical_oxdiff_formula         'C H O N Ce F Cl'
_reflns_odcompleteness_completeness 99.80
_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. Rigid bond restraints
 F9, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O8, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O9, C25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O10, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O11, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(F9) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F13) \\sim
Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F17) \\sim Ueq,
Uanis(F16) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F33) \\sim Ueq, Uanis(F32)
\\sim Ueq, Uanis(F31) \\sim Ueq, Uanis(F34) \\sim Ueq, Uanis(F36) \\sim Ueq,
Uanis(F35) \\sim Ueq, Uanis(F30) \\sim Ueq, Uanis(F28) \\sim Ueq, Uanis(F29)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(C19) \\sim
Ueq, Uanis(C25) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F32) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C21(H21), C26(H26), C31(H31), C42(H42), C43(H43), C54(H54),
 C59(H59), C64(H64)
4.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'