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_7046587
_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, C4 H10 O'
_chemical_formula_sum            'C31 H19 F18 Gd N2 O9'
_chemical_formula_weight         1062.73
_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                 98.929(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6200(3)
_cell_length_b                   22.9967(6)
_cell_length_c                   17.1078(4)
_cell_measurement_reflns_used    18136
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.1290
_cell_measurement_theta_min      2.9010
_cell_volume                     3738.86(18)
_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                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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    -28.00  94.00   1.00    1.60    --    5.00  72.00 -30.00  122
  2  \w      1.00  28.00   1.00    1.60    --    5.00  38.00-180.00   27
  3  \w    -17.00   9.00   1.00    1.60    --   -9.90 -72.00 -60.00   26
  4  \w     -9.00  63.00   1.00    1.60    --   -9.90  38.00  30.00   72
  5  \w    -43.00  79.00   1.00    1.60    --   -9.90  72.00 -90.00  122
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0347161000
_diffrn_orient_matrix_UB_12      -0.0137435000
_diffrn_orient_matrix_UB_13      -0.0347276000
_diffrn_orient_matrix_UB_21      -0.0255140000
_diffrn_orient_matrix_UB_22      0.0273845000
_diffrn_orient_matrix_UB_23      -0.0150406000
_diffrn_orient_matrix_UB_31      0.0609264000
_diffrn_orient_matrix_UB_32      0.0036175000
_diffrn_orient_matrix_UB_33      -0.0181297000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43077
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.410
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.918
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_description       block
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.096
_refine_diff_density_max         5.745
_refine_diff_density_min         -2.717
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8526
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0915
_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^)+(0.1510P)^2^+43.2990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2707
_refine_ls_wR_factor_ref         0.2793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7233
_reflns_number_total             8526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01262h2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7046585--7046591.cif.'
_cod_original_cell_volume        3738.87(18)
_cod_database_code               7046587
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C27 H9 O8 F18 Gd1'
_chemical_oxdiff_usercomment     SH01_015b
_cell_oxdiff_angle_alpha         89.996(2)
_cell_oxdiff_angle_beta          98.906(3)
_cell_oxdiff_angle_gamma         89.972(2)
_cell_oxdiff_length_a            9.6215(3)
_cell_oxdiff_length_b            22.9900(6)
_cell_oxdiff_length_c            17.1092(5)
_cell_oxdiff_measurement_reflns_used 18136
_cell_oxdiff_volume              3738.87(19)
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.509
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
 C5E-C3E = C4E-C3E
 1.51 with sigma of 0.02
 O9-C2E \\sim O9-C3E
 with sigma of 0.02
 C4E-C3E \\sim C5E-C3E \\sim C2E-C1E
 with sigma of 0.02
3. Others
 Fixed Sof: H3EA(0.6666) H3EB(0.6666) H3EC(0.33333) H3ED(0.33333) C4E(0.6666)
 H4EA(0.6666) H4EB(0.6666) H4EC(0.6666) C5E(0.33333) H5EA(0.33333)
 H5EB(0.33333) H5EC(0.33333)
4.a Secondary CH2 refined with riding coordinates:
 C2E(H2EA,H2EB), C3E(H3EA,H3EB), C3E(H3EC,H3ED)
4.b Me refined with riding coordinates:
 C1E(H1EA,H1EB,H1EC), C4E(H4EA,H4EB,H4EC), C5E(H5EA,H5EB,H5EC)
4.c 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)
;
_shelx_res_checksum              45997
_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 1.747
_oxdiff_exptl_absorpt_empirical_full_min 0.328