Aerobic oxygenation of α-methylene ketones under visible-light catalysed by a CeNi<sub>3</sub> complex with a macrocyclic tris(salen)-ligand.
Nagae, Haruki; Sakamoto, Kazutaka; Fujiwara, Sakiko; Schindler, Tobias; Kon, Yoshihiro; Sato, Kazuhiko; Okuda, Jun; Mashima, Kazushi; Chemical communications (Cambridge, England) 57 (2021) 11169–11172; doi:10.1039/d1cc04540g

data_7129013
_publ_section_title
;
 Aerobic oxygenation of \a-methylene ketones under visible-light catalysed
 by a CeNi<sub>3</sub> complex with a macrocyclic tris(salen)-ligand.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11169
_journal_page_last               11172
_journal_paper_doi               10.1039/d1cc04540g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C34 H30 Ce N6 Ni3 O10, C2 H3 O2'
_chemical_formula_sum            'C36 H33 Ce N6 Ni3 O12'
_chemical_formula_weight         1057.93
_chemical_melting_point_gt       573
_chemical_name_common            6CeNi
_chemical_name_systematic        CeNi3L(OAc)3
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_update_record
;
2021-08-16 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                62.578(3)
_cell_angle_beta                 75.394(4)
_cell_angle_gamma                77.110(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3694(5)
_cell_length_b                   17.4057(11)
_cell_length_c                   18.0006(13)
_cell_measurement_reflns_used    27.5
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2234.9(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  Rigaku_XtaLAB_P200_007
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1211
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            82021
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    2.305
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ABSCOR(Rigaaku,1995)
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       plate
_exptl_crystal_F_000             1058
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.303
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.131
_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     544
_refine_ls_number_reflns         10221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0836P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8432
_reflns_number_total             10221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04540g2.cif
_cod_data_source_block           6CeNi
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_chemical_melting_point' was changed to
'_chemical_melting_point_gt' since the value was specified as 'more
than' ('>') a certain temperature.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7129011--7129013.cif.
;
_cod_database_code               7129013
_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. Others
 Fixed Sof: O7(0.75) O8(0.75) O14(0.25) O13(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C21(H21A,H21B), C12(H12A,H12B), C2(H2A,H2B), C11(H11A,H11B),
 C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C20(H20), C13(H13), C23(H23), C28(H28), C27(H27), C3(H3), C7(H7),
 C10(H10), C8(H8), C17(H17), C18(H18)
3.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4586
_shelx_hkl_checksum              53896
_shelx_fab_checksum              11197
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id SKM3013
_olex2_submission_special_instructions 'No special instructions were received'