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_7122710
_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 N4 O8 Yb, 2(I), 2(C4 H8 O)'
_chemical_formula_sum            'C68 H96 I2 N4 O10 Yb'
_chemical_formula_weight         1556.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.716(7)
_cell_angle_beta                 75.423(6)
_cell_angle_gamma                78.241(7)
_cell_formula_units_Z            1
_cell_length_a                   10.9440(8)
_cell_length_b                   11.7197(12)
_cell_length_c                   15.4166(12)
_cell_measurement_reflns_used    27130
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      1.89
_cell_volume                     1757.8(3)
_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)
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      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
 266 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_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  0.0184
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13542
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.056
_diffrn_reflns_theta_min         1.892
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.27
_exptl_absorpt_correction_T_max  0.6348
_exptl_absorpt_correction_T_min  0.3980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.335
_exptl_crystal_size_min          0.206
_refine_diff_density_max         1.634
_refine_diff_density_min         -2.220
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6901
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0384P)^2^+3.0504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6211
_reflns_number_total             6901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08120d2.cif
_cod_data_source_block           txs253
_cod_database_code               7122710
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.463
_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
 O1B-C1B \\sim C1B-O2A
 with sigma of 0.005
 O2B-C1A \\sim C1A-O1A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C31A \\sim C32A \\sim C33A \\sim C34A: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
C31B \\sim C32B \\sim C33B \\sim C34B: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C31A, C32A, C33A, C34A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C31B, C32B, C33B, C34B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O2A, C1B, O1B, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: O1B(0.5) O2B(0.5) C1B(0.5) H27A(0.6) H27B(0.6) H27C(0.4) H27D(0.4)
 C28A(0.6) H28A(0.6) H28B(0.6) C28B(0.4) H28C(0.4) H28D(0.4) C29A(0.6)
 H29A(0.6) H29B(0.6) C29B(0.4) H29C(0.4) H29D(0.4) H30A(0.6) H30B(0.6)
 H30C(0.4) H30D(0.4) C31A(0.6) H31A(0.6) H31B(0.6) C31B(0.4) H31C(0.4)
 H31D(0.4) C32A(0.6) H32A(0.6) H32B(0.6) C32B(0.4) H32C(0.4) H32D(0.4)
 C33A(0.6) H33A(0.6) H33B(0.6) C33B(0.4) H33C(0.4) H33D(0.4) C34A(0.6)
 H34A(0.6) H34B(0.6) C34B(0.4) H34C(0.4) H34D(0.4) O1A(0.5) C1A(0.5) O2A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C27(H27C,H27D), C28A(H28A,H28B), C28B(H28C,H28D), C29A(H29A,H29B),
 C29B(H29C,H29D), C30(H30A,H30B), C30(H30C,H30D), C31A(H31A,H31B), C31B(H31C,
 H31D), C32A(H32A,H32B), C32B(H32C,H32D), C33A(H33A,H33B), C33B(H33C,H33D),
 C34A(H34A,H34B), C34B(H34C,H34D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C11(H11), C17(H17), C20(H20)
6.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              16978
_shelx_hkl_checksum              46048
_olex2_submission_special_instructions 'No special instructions were received'