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_7122709
_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         'C33 H48 I2 N2 O3 Yb, C4 H8 O'
_chemical_formula_sum            'C37 H56 I2 N2 O4 Yb'
_chemical_formula_weight         1019.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.494(4)
_cell_length_b                   19.122(4)
_cell_length_c                   22.718(5)
_cell_measurement_reflns_used    27986
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      1.77
_cell_volume                     8034(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 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
 113 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  0.0709
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37171
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.205
_diffrn_reflns_theta_min         1.775
_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    3.90
_exptl_absorpt_correction_T_max  0.3112
_exptl_absorpt_correction_T_min  0.2069
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.537
_exptl_crystal_size_mid          0.434
_exptl_crystal_size_min          0.379
_refine_diff_density_max         1.456
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         10812
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7964
_reflns_number_total             10812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08120d2.cif
_cod_data_source_block           txs202
_cod_database_code               7122709
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.319
_shelx_estimated_absorpt_t_min   0.228
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37A-C36A \\sim C36A-C35A \\sim C35A-C34A
 with sigma of 0.02
 O4A-C37A \\sim O4A-C34A
 with sigma of 0.02
 O4A-C36A \\sim O4A-C35A
 with sigma of 0.04
 C36A-C34A \\sim C37A-C35A
 with sigma of 0.04
 C37B-C36B \\sim C36B-C35B \\sim C35B-C34B
 with sigma of 0.02
 O4B-C37B \\sim O4B-C34B
 with sigma of 0.02
 O4B-C36B \\sim O4B-C35B
 with sigma of 0.04
 C36B-C34B \\sim C37B-C35B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O4A \\sim C34A \\sim C35A \\sim C36A \\sim C37A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
O4B \\sim C34B \\sim C35B \\sim C36B \\sim C37B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O4A, C34A, C35A, C36A, C37A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4B, C34B, C35B, C36B, C37B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O4B(0.5) C34B(0.5) H34A(0.5) H34B(0.5) C35B(0.5) H35A(0.5)
 H35B(0.5) C36B(0.5) H36A(0.5) H36B(0.5) C37B(0.5) H37A(0.5) H37B(0.5) O4A(0.5)
 C34A(0.5) H34C(0.5) H34D(0.5) C35A(0.5) H35C(0.5) H35D(0.5) C36A(0.5)
 H36C(0.5) H36D(0.5) C37A(0.5) H37C(0.5) H37D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34B(H34A,H34B), C35B(H35A,
 H35B), C36B(H36A,H36B), C37B(H37A,H37B), C34A(H34C,H34D), C35A(H35C,H35D),
 C36A(H36C,H36D), C37A(H37C,H37D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C10(H10), C16(H16), C19(H19)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C),
 C18(H18A,H18B,H18C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              58760
_shelx_hkl_checksum              95149
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'