Valence tautomerism in a cobalt-verdazyl coordination compound.
Fleming, Connor; Chung, Dorothy; Ponce, Servando; Brook, David J. R.; DaRos, Jeffrey; Das, Raja; Ozarowski, Andrew; Stoian, Sebastian A.; Chemical communications (Cambridge, England) 56 (2020) 4400–4403; doi:10.1039/d0cc01770a

data_7126278
_publ_section_title
;
 Valence tautomerism in a cobalt-verdazyl coordination compound.
;
_journal_issue                   32
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4400
_journal_page_last               4403
_journal_paper_doi               10.1039/d0cc01770a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C30 H30 Co N12 O2, F6 P, C H2 Cl2'
_chemical_formula_sum            'C31 H32 Cl2 Co F6 N12 O2 P'
_chemical_formula_weight         879.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-12
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-14 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2862(15)
_cell_length_b                   20.4254(12)
_cell_length_c                   21.7177(12)
_cell_measurement_reflns_used    9458
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.633
_cell_measurement_theta_min      2.252
_cell_volume                     4112.8(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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_temperature      150
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            151425
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.762
_diffrn_reflns_theta_min         1.652
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_correction_T_min  0.7962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1011 before and 0.0583 after correction.
The Ratio of minimum to maximum transmission is 0.9235.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_preparation
'From cobalt triflate and the ligand in acetonitrile'
_exptl_crystal_recrystallization_method dichloromethane/octane
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.697
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         9047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0528
_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^)+(0.1070P)^2^+2.9610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7798
_reflns_number_total             9047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01770a2.cif
_cod_data_source_block           sjsu011_0m
_cod_depositor_comments
'Adding full bibliography for 7126278--7126279.cif.'
_cod_database_code               7126278
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.944
_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. Shared sites
{N8, C17A}
{N10, C16A}
{C17, N8A}
{C16, N10A}
{C28, C28A}
3. Uiso/Uaniso restraints and constraints
Uanis(N8) = Uanis(C17A)
Uanis(N10) = Uanis(C16A)
Uanis(C17) = Uanis(N8A)
Uanis(C16) = Uanis(N10A)
Uanis(C28A) = Uanis(C28)
4. Others
 Sof(C28A)=Sof(H28A)=Sof(C17A)=Sof(C16A)=Sof(N10A)=Sof(N8A)=Sof(O2A)=Sof(C30A)=
 Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(N8)=Sof(C17)=Sof(N10)=Sof(C16)=Sof(O2)=Sof(C28)=Sof(H28)=Sof(C30)=
 Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C28(H28), C28A(H28A), C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
5.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C7(H7), C12(H12), C4(H4), C5(H5), C27(H27), C9(H9), C10(H10),
 C19(H19), C6(H6), C11(H11), C21(H21), C20(H20), C26(H26), C24(H24), C25(H25)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C30A(H30D,H30E,H30F)
;
_olex2_submission_special_instructions 'No special instructions were received'