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_7129012
_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         'C48 H52 Ce N6 O12 Zn3, H2 O, C H Cl3'
_chemical_formula_sum            'C49 H54 Ce Cl0.25 N6 O15 Zn3'
_chemical_formula_weight         1312.07
_chemical_melting_point_gt       573
_chemical_name_common            1CeZn
_chemical_name_systematic        CeZn3L(OAc)3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_update_record
;
2021-08-16 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.719(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2210(16)
_cell_length_b                   15.1088(19)
_cell_length_c                   32.186(4)
_cell_measurement_reflns_used    7257
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      4.1
_cell_volume                     5913.4(13)
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_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  0.1091
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            95190
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.536
_diffrn_reflns_theta_min         4.049
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    2.033
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ABSCOR(Rigaku,1995)
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       plate
_exptl_crystal_F_000             2649
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2 / hexane (vapor)'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.958
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         13546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0738
_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^)+(0.0001P)^2^+77.3862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9206
_reflns_number_total             13546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04540g2.cif
_cod_data_source_block           1CeZn
_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_original_cell_volume        5913(12)
_cod_database_code               7129012
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.792
_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) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: C2(0.5) H2(0.5) C1(0.5) H1(0.5) H3AA(0.5) H3AB(0.5) H3BC(0.5)
 H3BD(0.5) C5(0.5) H5A(0.5) H5B(0.5) C4(0.5) H4A(0.5) H4B(0.5) H6BC(0.5)
 H6BD(0.5) H6AA(0.5) H6AB(0.5) H7BC(0.5) H7BD(0.5) H7AA(0.5) H7AB(0.5) H18(0.5)
 H18A(0.5) H20C(0.5) H20D(0.5) H20A(0.5) H20B(0.5) H23A(0.5) H23B(0.5)
 H23C(0.5) H23D(0.5) C25(0.5) H25(0.5) C24(0.5) H24(0.5) H34A(0.5) H34(0.5)
 H36C(0.5) H36D(0.5) H39C(0.5) H39D(0.5) H39A(0.5) H39B(0.5) C40(0.5) H40(0.5)
 C41(0.5) H41(0.5) C21(0.5) H21A(0.5) H21B(0.5) C38(0.5) H38A(0.5) H38B(0.5)
 C22(0.5) H22A(0.5) H22B(0.5) C37(0.5) H37A(0.5) H37B(0.5) C8(0.5) H8(0.5)
 C9(0.5) H9(0.5)
3.a Free rotating group:
 O13(H13A,H13B)
3.b Ternary CH refined with riding coordinates:
 C2(H2), C1(H1), C18(H18), C18(H18A), C25(H25), C24(H24), C34(H34A), C34(H34),
 C40(H40), C41(H41), C8(H8), C9(H9), C56(H56)
3.c Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C5(H5A,H5B), C4(H4A,H4B), C6(H6BC,H6BD),
 C6(H6AA,H6AB), C7(H7BC,H7BD), C7(H7AA,H7AB), C19(H19A,H19B), C20(H20C,H20D),
 C20(H20A,H20B), C23(H23A,H23B), C23(H23C,H23D), C35(H35A,H35B), C36(H36A,H36B),
  C36(H36C,H36D), C39(H39C,H39D), C39(H39A,H39B), C21(H21A,H21B), C38(H38A,
 H38B), C22(H22A,H22B), C37(H37A,H37B)
3.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C17(H17), C26(H26), C29(H29), C30(H30),
 C33(H33), C42(H42), C45(H45), C46(H46), C49(H49)
3.e Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C53(H53A,H53B,H53C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              8645
_shelx_hkl_checksum              908
_shelx_fab_checksum              90053
_platon_squeeze_void_probe_radius 1.20
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id FJW3108
_olex2_submission_special_instructions 'No special instructions were received'