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_7126279
_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_absolute_configuration unk
_chemical_formula_moiety         'C30 H30 Co N12 O2, 2(F6 P)'
_chemical_formula_sum            'C30 H30 Co F12 N12 O2 P2'
_chemical_formula_weight         939.53
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7805(4)
_cell_length_b                   15.7805(4)
_cell_length_c                   15.4465(14)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    150
_cell_measurement_theta_max      40.2303
_cell_measurement_theta_min      3.7535
_cell_volume                     3846.6(4)
_computing_cell_refinement       'Bruker SAINT v8.37A'
_computing_data_collection       'Bruker APEX3 v2016.1.0'
_computing_data_reduction        'Bruker SAINT v8.37A'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  ALS_BL1131_post_07_2014
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.0333
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40042
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        38.315
_diffrn_reflns_theta_max         40.355
_diffrn_reflns_theta_min         2.654
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  0.8628
_exptl_absorpt_correction_T_min  0.7464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1057 before and 0.0467 after correction.
The Ratio of minimum to maximum transmission is 0.8651.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear greenish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       needle
_exptl_crystal_F_000             1900
_exptl_crystal_recrystallization_method 'diffuson of ether vapor into acetone'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 1428 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.401(3)
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+1.5100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3605
_reflns_number_total             3945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01770a2.cif
_cod_data_source_block           sjsu008a_0m
_cod_depositor_comments
'Adding full bibliography for 7126278--7126279.cif.'
_cod_database_code               7126279
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N4, C1A}
{C2, N2A}
{C1, N4A}
{N2, C2A}
{C13, C13A}
3. Uiso/Uaniso restraints and constraints
Uanis(N4) = Uanis(C1A)
Uanis(C2) = Uanis(N2A)
Uanis(C1) = Uanis(N4A)
Uanis(N2) = Uanis(C2A)
Uanis(C13) = Uanis(C13A)
4. Others
 Sof(O1A)=Sof(C1A)=Sof(N2A)=Sof(N4A)=Sof(C2A)=Sof(C14A)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C13A)=Sof(H13A)=1-FVAR(1)
 Sof(C2)=Sof(N4)=Sof(N2)=Sof(C1)=Sof(O1)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C13A(H13A)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C6(H6), C4(H4), C5(H5), C11(H11), C10(H10), C9(H9)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C14A(H14D,H14E,H14F), C15A(H15D,
 H15E,H15F)
;
_olex2_submission_special_instructions 'No special instructions were received'