Copper-promoted methylene C-H oxidation to a ketone derivative by O2.
Deville, Claire; McKee, Vickie; McKenzie, Christine J.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 709–719; doi:10.1039/c6dt03349k

data_7041504
_publ_section_title
;
 Copper-promoted methylene C-H oxidation to a ketone derivative by O2.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              709
_journal_page_last               719
_journal_paper_doi               10.1039/c6dt03349k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C72 H63 Fe3 N18 O6, 4(PF6), 2(C2 H6 O), 3(H2 O)'
_chemical_formula_sum            'C76 H81 F24 Fe3 N18 O11 P4'
_chemical_formula_weight         2170.01
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2016-11-25 deposited with the CCDC.
2016-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                91.302(3)
_cell_angle_beta                 113.159(3)
_cell_angle_gamma                111.623(3)
_cell_formula_units_Z            1
_cell_length_a                   13.0092(7)
_cell_length_b                   14.3276(7)
_cell_length_c                   15.0070(8)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.37
_cell_volume                     2344.3(2)
_computing_cell_refinement       'SAINT v.7.68a (Bruker, 2010)'
_computing_data_collection       'APEX2 v.2010.1-2 (Bruker Nonius, 2010)'
_computing_data_reduction        'SAINT v.7.68a (Bruker, 2010)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2008)'
_computing_publication_material  'PublCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice \w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48623
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.070
_diffrn_source                   'fine-focus sealed-tube'
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008, (Sheldrick, 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             1105
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         9548
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0748P)^2^+2.1981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7826
_reflns_number_total             9548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03349k2.cif
_cod_data_source_block           cm1378cd_sq
_cod_depositor_comments
'Adding full bibliography for 7041497--7041504.cif.'
_cod_database_code               7041504
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              31287
_shelx_fab_checksum              1547