Square-planar Co(iii) in {O<sub>4</sub>} coordination: large ZFS and reactivity with ROS.
Steele, Jennifer L.; Tahsini, Laleh; Sun, Chen; Elinburg, Jessica K.; Kotyk, Christopher M.; McNeely, James; Stoian, Sebastian A.; Dragulescu-Andrasi, Alina; Ozarowski, Andrew; Ozerov, M.; Krzystek, J.; Telser, Joshua; Bacon, Jeffrey W.; Golen, James A.; Rheingold, Arnold L.; Doerrer, Linda H.; Chemical communications (Cambridge, England) 54 (2018) 12045–12048; doi:10.1039/c8cc04464c

data_7122422
_publ_section_title
;
 Square-planar Co(iii) in {O<sub>4</sub>} coordination: large ZFS and
 reactivity with ROS.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12045
_journal_page_last               12048
_journal_paper_doi               10.1039/c8cc04464c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C12 Co F24 O4, C4 H12 N'
_chemical_formula_sum            'C16 H12 Co F24 N O4'
_chemical_formula_weight         797.20
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Light-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2017-10-12 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2160(8)
_cell_length_b                   20.2934(9)
_cell_length_c                   7.1911(4)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.497
_cell_measurement_theta_min      4.353
_cell_volume                     2512.4(2)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker Proteum-R'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_monochromator  Montel
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            14534
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        66.629
_diffrn_reflns_theta_max         66.629
_diffrn_reflns_theta_min         4.357
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    7.354
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_description       prism
_exptl_crystal_F_000             1560
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2229
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0650P)^2^+2.1450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2058
_reflns_number_total             2229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04464c2.cif
_cod_data_source_block           steele3_Compound_3
_cod_depositor_comments
'Adding full bibliography for 7122422--7122423.cif.'
_cod_database_code               7122422
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C2N = N1-C1N = N1-C3N = N1-C4N
 1.48 with sigma of 0.02
 C3N-C2N
 2.42 with sigma of 0.04
 C4N-C2N
 2.42 with sigma of 0.04
 C1N-C2N
 2.42 with sigma of 0.04
 C1N-C4N
 2.42 with sigma of 0.04
 C1N-C3N
 2.42 with sigma of 0.04
 C4N-C3N
 2.42 with sigma of 0.04
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N1(0.5) C2N(0.5) H2NA(0.5) H2NB(0.5) H2NC(0.5) C1N(0.5) H1NA(0.5)
 H1NB(0.5) H1NC(0.5) C3N(0.5) H3NA(0.5) H3NB(0.5) H3NC(0.5) C4N(0.5) H4NA(0.5)
 H4NB(0.5) H4NC(0.5)
5.a Idealised Me refined as rotating group:
 C2N(H2NA,H2NB,H2NC), C1N(H1NA,H1NB,H1NC), C3N(H3NA,H3NB,H3NC), C4N(H4NA,H4NB,
 H4NC)
;
_shelx_res_checksum              70212
_shelx_hkl_checksum              90391
_olex2_submission_special_instructions 'No special instructions were received'