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_7046585
_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 N2 O8 Y, C4 H10 O'
_chemical_formula_sum            'C31 H19 F18 N2 O9 Y'
_chemical_formula_weight         994.39
_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                 99.1760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6263(3)
_cell_length_b                   22.7963(8)
_cell_length_c                   17.0279(6)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.32
_cell_volume                     3688.9(2)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0313
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.322
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.727
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1028 before and 0.0482 after correction. The Ratio of minimum to maximum transmission is 0.7430. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       column
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.768
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         8416
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0890P)^2^+5.8620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6684
_reflns_number_total             8416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01262h2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7046585--7046591.cif.'
_cod_database_code               7046585
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.653
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O11-C2EA = O11-C3E = O10-C3E = O10-C2EB
 1.43 with sigma of 0.01
 C4E-C3E \\sim C2EA-C1EA \\sim C1EB-C2EB
 with sigma of 0.02
3. Others
 Fixed Sof: H3EC(0.5) H3ED(0.5) H3EA(0.5) H3EB(0.5) C1EA(0.5) H1EA(0.5)
 H1EB(0.5) H1EC(0.5) O10(0.5) C2EA(0.5) H2EA(0.5) H2EB(0.5) O11(0.5) C1EB(0.5)
 H1ED(0.5) H1EE(0.5) H1EF(0.5) C2EB(0.5) H2EC(0.5) H2ED(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C3E(H3EC,H3ED), C3E(H3EA,H3EB), C2EA(H2EA,H2EB), C2EB(H2EC,H2ED)
4.b Me refined with riding coordinates:
 C4E(H4EA,H4EB,H4EC), C1EA(H1EA,H1EB,H1EC), C1EB(H1ED,H1EE,H1EF)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C25(H25), C15(H15), C8(H8), C20(H20), C9(H9), C1(H1), C3(H3), C2(H2)
;
_shelx_res_checksum              577
_olex2_submission_special_instructions 'No special instructions were received'