The modular synthesis of rare earth-transition metal heterobimetallic complexes utilizing a redox-active ligand.
Hickson, James R.; Horsewill, Samuel J.; Bamforth, Christopher; McGuire, Jake; Wilson, Claire; Sproules, Stephen; Farnaby, Joy H.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10692–10701; doi:10.1039/c8dt01262h

data_7046586
_publ_section_title
;
 The modular synthesis of rare earth-transition metal heterobimetallic
 complexes utilizing a redox-active ligand.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10692
_journal_page_last               10701
_journal_paper_doi               10.1039/c8dt01262h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C27 H9 F18 Gd N2 O8, C7 H8'
_chemical_formula_sum            'C34 H17 F18 Gd N2 O8'
_chemical_formula_weight         1080.74
_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     dual
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-26 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.338(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9683(18)
_cell_length_b                   16.576(3)
_cell_length_c                   18.018(2)
_cell_measurement_reflns_used    2420
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.2240
_cell_measurement_theta_min      3.4910
_cell_volume                     3768.7(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -74.00 -48.00   0.50   28.00    --  -90.00  34.00-130.00   52
  2  \w    -42.00  -4.00   0.50   28.00    --  -90.00  34.00-130.00   76
  3  \w   -178.00-108.00   0.50   28.00    --  -90.00  34.00-130.00  140
  4  \w     39.00  65.00   0.50    7.00    --    0.00  34.00-130.00   52
  5  \w    -87.00  88.00   0.50    7.00    --    0.00  60.00-150.00  350
  6  \w    -82.00 -56.00   0.50    7.00    --    0.00  34.00-130.00   52
  7  \w    -19.00   6.00   0.50   28.00    --    5.00  34.00-130.00   50
  8  \w   -165.00-139.00   0.50   28.00    --  -90.00  60.00 120.00   52
  9  \w   -124.00 -97.00   0.50   28.00    --  -90.00  60.00 150.00   54
 10  \w   -172.00  -1.00   0.50   28.00    --  -90.00  29.00  90.00  342
 11  \w   -176.00-135.00   0.50   28.00    --  -90.00  29.00   0.00   82
 12  \w    -70.00 -44.00   0.50   28.00    --  -90.00  57.00 -30.00   52
 13  \w   -113.00  -8.00   0.50   28.00    --  -90.00  29.00   0.00  210
 14  \w    -44.00 -10.00   0.50   28.00    --  -90.00  60.00 150.00   68
 15  \w   -132.00  -2.00   0.50   28.00    --  -90.00  60.00 120.00  260
 16  \w    -69.00 -20.00   0.50   28.00    --  -90.00  29.00 -60.00   98
 17  \w   -161.00-108.00   0.50   28.00    --  -90.00  29.00 -60.00  106
 18  \w    -92.00 -66.00   0.50   28.00    --  -90.00  60.00 150.00   52
 19  \w   -178.00-100.00   0.50   28.00    --  -90.00  57.00 -30.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1075678000
_diffrn_orient_matrix_UB_12      0.0403295000
_diffrn_orient_matrix_UB_13      -0.0343481000
_diffrn_orient_matrix_UB_21      -0.0447406000
_diffrn_orient_matrix_UB_22      -0.0339650000
_diffrn_orient_matrix_UB_23      0.0656390000
_diffrn_orient_matrix_UB_31      0.0363981000
_diffrn_orient_matrix_UB_32      0.0766074000
_diffrn_orient_matrix_UB_33      0.0471983000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2149
_diffrn_reflns_av_unetI/netI     0.2252
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24190
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         3.502
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.311
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         6759
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.2532
_refine_ls_R_factor_gt           0.1180
_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^)+(0.1980P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2952
_refine_ls_wR_factor_ref         0.3797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2780
_reflns_number_total             6759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01262h2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7046585--7046591.cif.'
_cod_original_cell_volume        3768.9(10)
_cod_database_code               7046586
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C27 H9 N2 O8 F18 Gd'
_chemical_oxdiff_usercomment     SHOI-015
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.569
_reflns_odcompleteness_completeness 97.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
 F17A-C27 \\sim F17-C27 \\sim F16A-C27 \\sim F16-C27 \\sim F18A-C27 \\sim
F18-C27
 with sigma of 0.02
 F12A-C22 \\sim F11A-C22 \\sim F12-C22 \\sim F10-C22 \\sim F11-C22 \\sim
F10A-C22 \\sim C23-F13 \\sim C23-
 F15 \\sim C23-F14 \\sim F17-C27 \\sim F18-C27 \\sim F16-C27 \\sim F13-C23
\\sim F14-C23 \\sim F15-C23 ~
 C23-F14A \\sim C23-F13A \\sim C23-F15A
 with sigma of 0.02
 F18-F16 \\sim F17-F16 \\sim F18-F17 \\sim F18A-F16A \\sim F18A-F17A \\sim
F16A-F17A \\sim F13-F15 ~
 F13-F14 \\sim F15-F14 \\sim F14A-F13A \\sim F14A-F15A \\sim F13A-F15A
 with sigma of 0.02
3. Others
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(2)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(2)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
 Fixed Sof: C2S(0.5) H2S(0.5) C3S(0.5) H3S(0.5) C4S(0.5) H4S(0.5) C5S(0.5)
 H5S(0.5) C6S(0.5) H6S(0.5) C1S(0.5) C7S(0.5) H7SA(0.5) H7SB(0.5) H7SC(0.5)
 C3T(0.5) H3T(0.5) C2T(0.5) H2T(0.5) C1T(0.5) C6T(0.5) H6T(0.5) C5T(0.5)
 H5T(0.5) C4T(0.5) H4T(0.5) C7T(0.5) H7TA(0.5) H7TB(0.5) H7TC(0.5)
4.a Me refined with riding coordinates:
 C7S(H7SA,H7SB,H7SC), C7T(H7TA,H7TB,H7TC)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C20(H20),
 C25(H25), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C3T(H3T), C2T(H2T),
  C6T(H6T), C5T(H5T), C4T(H4T)
4.c Fitted hexagon refined as free rotating group:
 C2S(C3S,C4S,C5S,C6S,C1S), C3T(C2T,C1T,C6T,C5T,C4T)
;
_shelx_res_checksum              92856
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.373
_oxdiff_exptl_absorpt_empirical_full_min 0.295