Selective and catalytic carbon dioxide and heteroallene activation mediated by cerium N-heterocyclic carbene complexes.
Arnold, Polly L.; Kerr, Ryan W. F.; Weetman, Catherine; Docherty, Scott R.; Rieb, Julia; Cruickshank, Faye L.; Wang, Kai; Jandl, Christian; McMullon, Max W.; Pöthig, Alexander; Kühn, Fritz E; Smith, Andrew D.; Chemical science 9 (2018) 8035–8045; doi:10.1039/c8sc03312a

data_1549910
_publ_section_title
;
 Selective and catalytic carbon dioxide and heteroallene activation
 mediated by cerium N-heterocyclic carbene complexes.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              8035
_journal_page_last               8045
_journal_paper_doi               10.1039/c8sc03312a
_journal_volume                  9
_journal_year                    2018
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C56 H94 Br4 Ce2 Li2 N6 O4, C6 H6'
_chemical_formula_sum            'C62 H100 Br4 Ce2 Li2 N6 O4'
_chemical_formula_weight         1607.20
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2018-07-15 deposited with the CCDC.
2018-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.155(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0830(3)
_cell_length_b                   17.4883(2)
_cell_length_c                   15.0209(2)
_cell_measurement_reflns_used    19039
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.5410
_cell_measurement_theta_min      3.5830
_cell_volume                     3652.34(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'
_computing_structure_refinement
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_structure_solution
'SHELXT (Sheldrick, 2015), OLEX2 (Dolomanov, 2009)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            77453
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.462
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.584
_exptl_crystal_size_mid          0.407
_exptl_crystal_size_min          0.171
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         7464
_refine_ls_number_restraints     537
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0367P)^2^+8.5891P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                6117
_reflns_number_total             7464
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c8sc03312a2.cif
_cod_data_source_block           p17026
_cod_depositor_comments
'Adding full bibliography for 1549909--1549914.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1549910
_oxdiff_exptl_absorpt_empirical_full_min 0.750
_oxdiff_exptl_absorpt_empirical_full_max 1.689
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              67006