Light-induced O<sub>2</sub>-dependent aliphatic carbon-carbon (C-C) bond cleavage in bipyridine-ligated Co(II) chlorodiketonate complexes.
Anderson, Stephen N.; Elsberg, Josiah G. D.; Berreau, Lisa M.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt03727k

data_7712567
_publ_section_title
;
 Light-induced O<sub>2</sub>-dependent aliphatic carbon-carbon (C-C) bond
 cleavage in bipyridine-ligated Co(II) chlorodiketonate complexes.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt03727k
_journal_year                    2023
_chemical_formula_moiety         'C24 H22 Co N6, 2(Cl O4)'
_chemical_formula_sum            'C24 H22 Cl2 Co N6 O8'
_chemical_formula_weight         652.30
_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     dual
_audit_creation_date             2022-08-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-12 deposited with the CCDC.	2023-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                82.304(4)
_cell_angle_beta                 83.219(4)
_cell_angle_gamma                61.217(7)
_cell_formula_units_Z            2
_cell_length_a                   10.0272(8)
_cell_length_b                   10.2270(6)
_cell_length_c                   15.4354(6)
_cell_measurement_reflns_used    8610
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.2270
_cell_measurement_theta_min      2.2760
_cell_volume                     1372.19(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.948
_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     -5.00  34.00   0.50    6.16    --   20.00  54.00 170.30   78
  2  \w     71.00  96.00   0.50    6.16    --   20.00  54.00 170.30   50
  3  \w    -71.00 -17.00   0.50    6.16    --   20.00  54.00  30.00  108
  4  \w    -12.00  39.00   0.50    6.16    --   20.00  54.00  30.00  102
  5  \w     54.00 110.00   0.50    6.16    --   20.00  54.00  30.00  112
  6  \w    -71.00 110.00   0.50    6.16    --   20.00  54.00 -90.00  362
  7  \w    -69.00 -19.00   0.50    6.16    --   20.00  54.00 120.00  100
  8  \w     23.00  49.00   0.50    6.16    --   20.00  54.00 120.00   52
  9  \w     66.00 100.00   0.50    6.16    --   20.00  54.00 120.00   68
 10  \w    -35.00   9.00   0.50    6.16    --   20.00  54.00-120.00   88
 11  \w    -69.00  67.00   0.50    6.16    --   20.00  54.00 -30.00  272
 12  \w    -69.00  11.00   0.50    6.16    --   20.00  54.00  90.00  160
 13  \w     82.00 107.00   0.50    6.16    --   20.00  54.00  90.00   50
 14  \w    -16.00   9.00   0.50    6.16    --   20.00  54.00   0.00   50
 15  \w     53.00  78.00   0.50    6.16    --   20.00  54.00   0.00   50
 16  \w    -59.00 -34.00   0.50    6.16    --   20.00  54.00  60.00   50
 17  \w     40.00  65.00   0.50    6.16    --   20.00  54.00  60.00   50
 18  \w    -72.00  47.00   0.50    6.16    --   20.00  54.00-150.00  238
 19  \w    -66.00 -40.00   0.50    6.16    --   20.00  54.00 170.30   52
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0558082000
_diffrn_orient_matrix_UB_12      -0.0728784000
_diffrn_orient_matrix_UB_13      0.0146869000
_diffrn_orient_matrix_UB_21      -0.0521574000
_diffrn_orient_matrix_UB_22      -0.0275727000
_diffrn_orient_matrix_UB_23      -0.0022334000
_diffrn_orient_matrix_UB_31      0.0265316000
_diffrn_orient_matrix_UB_32      -0.0154916000
_diffrn_orient_matrix_UB_33      -0.0440198000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25701
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.549
_diffrn_reflns_theta_min         2.281
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       prism
_exptl_crystal_F_000             666
_exptl_crystal_preparation
'Cobalt(II) hexahydrate perchlorate in acetonitrile with 2 eq of bpy stirred for 30 min.'
_exptl_crystal_recrystallization_method
'Slow diffusion with diethylether and acetonitrile'
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0382P)^2^+0.4308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6251
_reflns_number_total             7973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03727k2.cif
_cod_data_source_block           finalizetake3
_cod_database_code               7712567
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co1 Cl2 O8 N6 C24 H22'
_reflns_odcompleteness_completeness 99.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C14(H14), C3(H3), C4(H4), C20(H20), C2(H2), C1(H1), C7(H7),
 C11(H11), C12(H12), C9(H9), C18(H18), C10(H10), C8(H8), C13(H13), C19(H19)
1.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              48875
_shelx_hkl_checksum              1378
_ins_header
;
TITL Finalize Take 3 in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  10.027216  10.226966  15.435400  82.3040  83.2195  61.2168
ZERR    2.00   0.000759   0.000635   0.000609   0.0041   0.0045   0.0070
LATT  1
SFAC C H N O Cl Co
UNIT 48.00 44.00 12.00 16.00 4.00 2.00
TREF
HKLF 4
END
;
_olex2_exptl_crystal_mounting_method 'Loop with paraton oil'
_olex2_submission_original_sample_id '[(bpy)2Co(II)(CH3CN)2](ClO4)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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.070
_oxdiff_exptl_absorpt_empirical_full_min 0.966