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_7712566
_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_absolute_configuration ad
_chemical_formula_moiety
'Cl O4, 0.5(C4 H10 O), C37 H30 Cl Co N4 O2, 0.5(C2 H3 N)'
_chemical_formula_sum            'C40 H36.5 Cl2 Co N4.5 O6.5'
_chemical_formula_weight         814.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4753(12)
_cell_length_b                   17.7824(9)
_cell_length_c                   19.6340(12)
_cell_measurement_reflns_used    9190
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.04
_cell_volume                     7497.9(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon-100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            96371
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         2.975
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0506 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.9435.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       prism
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.472(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         17244
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0485P)^2^+3.3408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                15087
_reflns_number_total             17244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03727k2.cif
_cod_data_source_block           lb15
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C40 H36.50 Cl2 Co N4.50 O6.50'
_cod_database_code               7712566
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.858
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52769
 0.47231
2.a Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C5S(H5SA,H5SB)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C8A(H8A), C9A(H9A),
 C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A), C17A(H17A),
 C18A(H18A), C19A(H19A), C20A(H20A), C26A(H26A), C27A(H27A), C29A(H29A),
 C30A(H30A), C31A(H31A), C32A(H32A), C34A(H34A), C35A(H35A), C1B(H1B), C2B(H2B),
  C3B(H3B), C4B(H4B), C7B(H7B), C8B(H8B), C9B(H9B), C10B(H10B), C11B(H11B),
 C12B(H12B), C13B(H13B), C14B(H14B), C17B(H17B), C18B(H18B), C19B(H19B),
 C20B(H20B), C26B(H26B), C27B(H27B), C29B(H29B), C30B(H30B), C31B(H31B),
 C32B(H32B), C34B(H34B), C35B(H35B)
2.c Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,H6SC), C36A(H36A,H36B,H36C), C37A(H37A,
 H37B,H37C), C36B(H36D,H36E,H36F), C37B(H37D,H37E,H37F), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              33337
_shelx_hkl_checksum              12366
_olex2_submission_original_sample_id 'Complex 9'
_olex2_submission_special_instructions 'No special instructions were received'