Copper(II)-photocatalyzed decarboxylative oxygenation of carboxylic acids.
Reichle, Alexander; Sterzel, Hannes; Kreitmeier, Peter; Fayad, Remi; Castellano, Felix N.; Rehbein, Julia; Reiser, Oliver; Chemical communications (Cambridge, England) 58 (2022) 4456–4459; doi:10.1039/d2cc00570k

data_7129719
_publ_section_title
;
 Copper(II)-photocatalyzed decarboxylative oxygenation of carboxylic
 acids.
;
_journal_issue                   28
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4456
_journal_page_last               4459
_journal_paper_doi               10.1039/d2cc00570k
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C32 H30 Cu N2 O6'
_chemical_formula_sum            'C32 H30 Cu N2 O6'
_chemical_formula_weight         602.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-28
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2022-01-25 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.289(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.6472(6)
_cell_length_b                   16.1411(4)
_cell_length_c                   13.7447(3)
_cell_measurement_reflns_used    6198
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.6690
_cell_measurement_theta_min      4.2840
_cell_volume                     5513.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.37b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -65.00  30.00   1.00   20.00    --  -42.68  37.00 -30.00   95
  2  \w   -117.00 -11.00   1.00   20.00    --  -42.68 -77.00  30.00  106
  3  \w     32.00  69.00   1.00   60.00    --  106.63 -30.00-150.00   37
  4  \w     35.00  77.00   1.00   60.00    --  106.63 -45.00 -30.00   42
  5  \w     79.00 158.00   1.00   60.00    --  106.63  61.00 -60.00   79
  6  \w     33.00 138.00   1.00   60.00    --  106.63 -77.00 -60.00  105
  7  \w     83.00 158.00   1.00   60.00    --  106.63  30.00  60.00   75
  8  \w     25.00 109.00   1.00   60.00    --  106.63 -94.00-180.00   84
  9  \w     32.00  69.00   1.00   60.00    --  106.63 -30.00  60.00   37
 10  \w   -117.00 -11.00   1.00   20.00    --  -42.68 -77.00-150.00  106
 11  \w    -27.00  69.00   1.00   20.00    --   42.68 -57.00  60.00   96
 12  \w     83.00 140.00   1.00   60.00    --  106.63  30.00 150.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0082085000
_diffrn_orient_matrix_UB_12      -0.0899038000
_diffrn_orient_matrix_UB_13      0.0306520000
_diffrn_orient_matrix_UB_21      0.0519058000
_diffrn_orient_matrix_UB_22      0.0057414000
_diffrn_orient_matrix_UB_23      0.0848477000
_diffrn_orient_matrix_UB_31      -0.0328636000
_diffrn_orient_matrix_UB_32      0.0314873000
_diffrn_orient_matrix_UB_33      0.0724333000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14926
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.143
_diffrn_reflns_theta_min         3.265
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.37b (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       plate
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0607P)^2^+3.9756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4303
_reflns_number_total             5395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00570k2.cif
_cod_data_source_block           s019
_cod_depositor_comments
'Adding full bibliography for 7129719--7129722.cif.'
_cod_database_code               7129719
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C32 H30 Cu N2 O6'
_chemical_oxdiff_usercomment     Reichle_Reiser_AR164-2
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C3(H3), C30(H30), C21(H21), C14(H14), C20(H20), C31(H31),
 C4(H4), C16(H16), C13(H13), C7(H7), C17(H17), C6(H6)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C18(H18A,H18B,H18C), C1(H1A,H1B,H1C), C0AA(H0AA,H0AB,H0AC)
;
_olex2_date_sample_data_collection 2019-01-25
_olex2_date_sample_submission    2019-01-25
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems CryoStream 700'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_original_sample_id AR164-2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.462
_oxdiff_exptl_absorpt_empirical_full_min 0.766