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_7046591
_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         'C37 H14 F18 N2 O8 V Y'
_chemical_formula_sum            'C37 H19 F18 N2 O8 V Y'
_chemical_formula_weight         1101.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_symmetry_space_group_name_Hall  'P -2ac -2n'
_symmetry_space_group_name_H-M   'P n 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-26
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0879(7)
_cell_length_b                   14.8963(9)
_cell_length_c                   19.6006(12)
_cell_measurement_reflns_used    6096
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.334
_cell_measurement_theta_min      2.244
_cell_volume                     4113.3(4)
_computing_cell_refinement       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28166
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.488
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0600 before and 0.0479 after correction. The Ratio of minimum to maximum transmission is 0.8741. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       shard
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 1728 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         6898
_refine_ls_number_restraints     995
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1260P)^2^+8.1630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2180
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4805
_reflns_number_total             6898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01262h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7046585--7046591.cif.'
_cod_database_code               7046591
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.730
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.48(3)
 0.52(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 F2-C13 = F1-C13 = F3-C13 = F4-C17 = F5-C17 = F6-C17 = F9-C18A = F8-C18A = F8A-
 C18A = F7-C18A = F7A-C18A = F9A-C18A = F10A-C22A = F13-C22A = F13-C23 = F14-
 C23 = F11A-C22A = F15-C23 = F17A-C22 = F11-C22 = F18A-C22 = F12-C22 = F16A-C22
 = F10-C22 = F13A-C23A = F14A-C23A = F15A-C23A = F17-C27 = F16-C27 = F18-C27
 1.33 with sigma of 0.02
 C37-C38 = C34-C38 = C34-C39 = C39-C40 = C37-C40 = C37-C36 = C33-C37 = C34-C33
 = C34-C35 = C36-C35
 1.42 with sigma of 0.01
 C31-C30 \\sim C29-C30 \\sim C29-C28 \\sim C32-C28 \\sim C31-C32
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F4-F5 \\sim F4-F6 \\sim F5-F6 \\sim F7-F8
\\sim F7-F9 \\sim F8-F9 \\sim F10-
 F11 \\sim F10-F12 \\sim F11-F12 \\sim F13-F14 \\sim F13-F15 \\sim F14-F15
\\sim F16-F17 \\sim F16-F18 ~
 F17-F18 \\sim F7A-F8A \\sim F7A-F9A \\sim F8A-F9A \\sim F16A-F17A \\sim
F16A-F18A \\sim F17A-F18A ~
 F13-F10A \\sim F13-F11A \\sim F10A-F11A \\sim F13A-F14A \\sim F13A-F15A \\sim
F14A-F15A
 with sigma of 0.02
4. Restrained planarity
 O8, C24A, C25A, C26A, O6, C22
 with sigma of 0.1
 C33, C34, C35, C36, C37
 with sigma of 0.1
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C38)=Sof(C39)=Sof(C40)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(C22A)=
 Sof(C23A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=
 Sof(F10A)=Sof(F11A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F17A)=
 Sof(F18A)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=
 Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(C23)=Sof(C24)=Sof(C25)=Sof(H25)=
 Sof(C26)=Sof(C27)=Sof(C33)=Sof(C35)=Sof(C36)=Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
7.a 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), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C20A(H20A),
 C25A(H25A)
;
_shelx_res_checksum              17387
_olex2_submission_special_instructions 'No special instructions were received'