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_7221924
_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 Gd N4 O11)'
_chemical_formula_sum            'C66 H58 F36 Gd2 N8 O22'
_chemical_formula_weight         2313.70
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-21
_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                90
_cell_angle_beta                 108.287(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.7235(10)
_cell_length_b                   12.6890(3)
_cell_length_c                   23.8780(7)
_cell_measurement_reflns_used    6691
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.6280
_cell_measurement_theta_min      3.7440
_cell_volume                     8551.0(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5479
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega -114.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4301  -57.0000 -120.0000 103

  2 omega  -93.00  -66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4301  125.0000 -150.0000 27

  3 omega  -50.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4301   38.0000   30.0000 85

  4 omega   36.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.4301 -125.0000 -180.0000 48

  5 omega   30.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000  120.0000 48

  6 omega   33.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -36.0000  170.0000 51

  7 omega   41.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -94.0000 -150.0000 57

  8 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064   30.0000  -60.0000 95

  9 omega   44.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -45.0000  -30.0000 52

 10 omega   99.00  175.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  125.0000 -150.0000 76

 11 omega   63.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -45.0000 -120.0000 27

 12 omega   45.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -45.0000   60.0000 53
;
_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      -0.0046318000
_diffrn_orient_matrix_UB_12      -0.0199516000
_diffrn_orient_matrix_UB_13      -0.0652146000
_diffrn_orient_matrix_UB_21      0.0493394000
_diffrn_orient_matrix_UB_22      -0.0520194000
_diffrn_orient_matrix_UB_23      0.0188401000
_diffrn_orient_matrix_UB_31      -0.0229335000
_diffrn_orient_matrix_UB_32      -0.1078157000
_diffrn_orient_matrix_UB_33      0.0029792000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.1142
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32652
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.718
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.319
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34008
_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            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       block
_exptl_crystal_F_000             4552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.968
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1233
_refine_ls_number_reflns         15270
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1080P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.2168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9546
_reflns_number_total             15270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra13386f2.cif
_cod_data_source_block           a141223a
_cod_original_cell_volume        8551.1(4)
_cod_database_code               7221924
_audit_block_doi                 10.5517/cc1jbk2h
_reflns_odcompleteness_completeness 99.95
_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
 F1-C24
 1.35 with sigma of 0.02
 F3'-C24
 1.35 with sigma of 0.02
 F3-C24
 1.35 with sigma of 0.02
 F2-C24
 1.35 with sigma of 0.02
 F2'-C24
 1.35 with sigma of 0.02
 F1'-C24
 1.35 with sigma of 0.02
 F3-F1 \\sim F1-F2
 with sigma of 0.01
 F1-F2 \\sim F2-F3
 with sigma of 0.01
 F2-F3 \\sim F3-F1
 with sigma of 0.01
 F1'-F2' \\sim F2'-F3'
 with sigma of 0.01
 F2'-F3' \\sim F3'-F1'
 with sigma of 0.01
 F3'-F1' \\sim F1'-F2'
 with sigma of 0.01
3. Rigid bond restraints
 O13, N7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(F12) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F3') \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(F2) = Uanis(F2')
Uanis(F3) = Uanis(F3')
Uanis(F1) = Uanis(F1')
5. Others
 Sof(F1')=Sof(F2')=Sof(F3')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C21(H21), C26(H26), C31(H31), C38(H38), C39(H39), C54(H54),
 C59(H59), C64(H64)
6.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C14(H14a,H14b,
 H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C18(H18a,
 H18b,H18c), C44(H44a,H44b,H44c), C45(H45a,H45b,H45c), C46(H46a,H46b,H46c),
 C47(H47a,H47b,H47c), C48(H48a,H48b,H48c), C49(H49a,H49b,H49c), C50(H50a,H50b,
 H50c), C51(H51a,H51b,H51c)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2014-12-23
_olex2_submission_special_instructions 'No special instructions were received'