Access to divalent lanthanide NHC complexes by redox-transmetallation from silver and CO2 insertion reactions
Simler, Thomas; Feuerstein, Thomas J.; Yadav, Ravi; Gamer, Michael T.; Roesky, Peter W.; Chemical Communications  (2019) –; doi:10.1039/C8CC08120D

data_7122708
_publ_section_title
;
 Access to divalent lanthanide NHC complexes by redox-transmetallation
 from silver and CO2 insertion reactions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08120D
_journal_year                    2019
_chemical_formula_moiety         'C60 H80 Eu N4 O8, 2(I), 2(C4 H8 O)'
_chemical_formula_sum            'C68 H96 Eu I2 N4 O10'
_chemical_formula_weight         1535.24
_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             2018-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-16 deposited with the CCDC.
2018-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.780(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7081(6)
_cell_length_b                   24.238(3)
_cell_length_c                   16.4401(12)
_cell_measurement_reflns_used    15551
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.38
_cell_volume                     3408.7(5)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_details
;
 428 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.1044
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15730
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.566
_diffrn_reflns_theta_min         2.381
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.88
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1562
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.022
_refine_diff_density_max         3.914
_refine_diff_density_min         -2.880
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         8042
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0864
_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^)+(0.1432P)^2^+28.8525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2148
_refine_ls_wR_factor_ref         0.2802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4798
_reflns_number_total             8042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08120d2.cif
_cod_data_source_block           txs191-co2
_cod_database_code               7122708
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.623
_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
 H10B-H31D
 2.1 with sigma of 0.01
3. Rigid body (RIGU) restrains
 O4A, C27A, C28A, C29A, C30A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O4B, C27B, C28B, C29B, C30B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O6, C31A, C34A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C5, C6, C8, C9, C11, C12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O6, C31B, C34B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: O4A(0.5) O4B(0.5) C27A(0.5) H27A(0.5) H27B(0.5) C27B(0.5)
 H27C(0.5) H27D(0.5) C28A(0.5) H28A(0.5) H28B(0.5) C28B(0.5) H28C(0.5)
 H28D(0.5) C29A(0.5) H29A(0.5) H29B(0.5) C29B(0.5) H29C(0.5) H29D(0.5)
 C30A(0.5) H30A(0.5) H30B(0.5) C30B(0.5) H30C(0.5) H30D(0.5) C31A(0.6)
 H31A(0.6) H31B(0.6) C31B(0.4) H31C(0.4) H31D(0.4) H32A(0.6) H32B(0.6)
 H32C(0.4) H32D(0.4) H33A(0.6) H33B(0.6) H33C(0.4) H33D(0.4) C34A(0.6)
 H34A(0.6) H34B(0.6) C34B(0.4) H34C(0.4) H34D(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27A(H27A,
 H27B), C27B(H27C,H27D), C28A(H28A,H28B), C28B(H28C,H28D), C29A(H29A,H29B),
 C29B(H29C,H29D), C30A(H30A,H30B), C30B(H30C,H30D), C31A(H31A,H31B), C31B(H31C,
 H31D), C32(H32A,H32B), C32(H32C,H32D), C33(H33A,H33B), C33(H33C,H33D),
 C34A(H34A,H34B), C34B(H34C,H34D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C11(H11), C17(H17), C20(H20)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              10465
_shelx_hkl_checksum              75154
_olex2_submission_special_instructions 'No special instructions were received'