Predicting valence tautomerism in diverse cobalt-dioxolene complexes: elucidation of the role of ligands and solvent.
M Zahir, F Zahra; Hay, Moya A.; Janetzki, Jett T.; Gable, Robert W.; Goerigk, Lars; Boskovic, Colette; Chemical science 15 (2024) 5694–5710; doi:10.1039/d3sc04493a

data_1571224
_publ_section_title
;
 Predicting valence tautomerism in diverse cobalt-dioxolene complexes:
 elucidation of the role of ligands and solvent.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              5694
_journal_page_last               5710
_journal_paper_doi               10.1039/d3sc04493a
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H26 Co N4 O2, C24 H20 B'
_chemical_formula_sum            'C50 H46 B Co N4 O2'
_chemical_formula_weight         804.65
_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             2023-05-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-08 deposited with the CCDC.	2024-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.872(6)
_cell_length_b                   9.931(2)
_cell_length_c                   27.754(6)
_cell_measurement_reflns_used    5748
_cell_measurement_temperature    271.59(2)
_cell_measurement_theta_max      19.99
_cell_measurement_theta_min      2.17
_cell_volume                     8233(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      270.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'Dectris Eiger2 9M'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            96159
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         29.232
_diffrn_reflns_theta_min         1.363
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Plate like flakes'
_exptl_crystal_F_000             3376
_exptl_crystal_recrystallization_method
'grown by solvent diffusion of hexane into dichloromethane'
_exptl_crystal_size_max          0.009
_exptl_crystal_size_mid          0.004
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.371(16)
_refine_ls_extinction_coef       0.0039(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1062
_refine_ls_number_reflns         19053
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0693P)^2^+1.9694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.821
_reflns_number_gt                14024
_reflns_number_total             19053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04493a3.cif
_cod_data_source_block           zz1-006-dcm-hex-270-x
_cod_depositor_comments
'Adding full bibliography for 1571222--1571238.cif.'
_cod_database_code               1571224
_shelx_shelxl_version_number     2019/3
_exptl_absorpt_special_details
;
XDS does not report the values of _exptl_absorpt_correction_T_min and
_exptl_absorpt_correction_T_max.  Even though the data was processed by XDS
the values of the absorption corrections reported by SADABS are reported.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.629(16)
 0.371(16)
2. 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
3. Restrained distances
 C18B-C26C
 1.5 with sigma of 0.001
4. Rigid body (RIGU) restrains
 C5B, C4B, C6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H7B)=Sof(C26C)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(H18B)=Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C13B(H13A,H13B), C13A(H13C,H13D), C12B(H12A,H12B), C19A(H19C,H19D), C19B(H19A,
 H19B), C12A(H12C,H12D)
6.b Aromatic/amide H refined with riding coordinates:
 C17B(H17B), C32B(H32B), C42B(H42B), C31B(H31B), C46A(H46A), C38B(H38B),
 C43B(H43B), C29A(H29A), C24A(H24A), C16B(H16B), C44B(H44B), C21A(H21A),
 C28A(H28A), C15A(H15A), C45B(H45B), C34A(H34A), C38A(H38A), C44A(H44A),
 C49B(H49B), C37B(H37B), C30A(H30A), C36B(H36B), C46B(H46B), C30B(H30B),
 C10A(H10A), C43A(H43A), C36A(H36A), C35B(H35B), C32A(H32A), C17A(H17A),
 C48B(H48B), C47A(H47A), C3B(H3B), C34B(H34B), C9A(H9A), C18B(H18B), C50A(H50A),
  C37A(H37A), C41B(H41B), C15B(H15B), C31A(H31A), C40B(H40B), C16A(H16A),
 C28B(H28B), C23B(H23B), C22A(H22A), C29B(H29B), C49A(H49A), C9B(H9B),
 C10B(H10B), C47B(H47B), C4B(H4B), C6A(H6A), C48A(H48A), C3A(H3A), C6B(H6B),
 C4A(H4A), C8B(H8B), C7B(H7B), C35A(H35A), C40A(H40A), C5A(H5A), C42A(H42A),
 C8A(H8A), C5B(H5B), C21B(H21B), C23A(H23A), C22B(H22B), C41A(H41A)
6.c Idealised Me refined as rotating group:
 C25A(H25D,H25E,H25F), C25B(H25A,H25B,H25C), C26A(H26G,H26H,H26I), C26B(H26A,
 H26B,H26C), C26C(H26D,H26E,H26F)
;
_shelx_res_checksum              95041
_olex2_submission_special_instructions 'No special instructions were received'