Hydrogen atom abstraction as a synthetic route to a square planar Co<sup>II</sup> complex with a redox-active tetradentate PNNP ligand.
Miller, Justin D.; Walsh, Mitchell M.; Lee, Kyounghoon; Moore, Curtis E.; Thomas, Christine M.; Chemical science 15 (2024) 15311–15320; doi:10.1039/d4sc03364g

data_1572437
_publ_section_title
;
 Hydrogen atom abstraction as a synthetic route to a square planar
 Co<sup>II</sup> complex with a redox-active tetradentate PNNP ligand.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              15311
_journal_page_last               15320
_journal_paper_doi               10.1039/d4sc03364g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C50 H54 Co K N2 O6 P2, C6 H6'
_chemical_formula_sum            'C56 H60 Co K N2 O6 P2'
_chemical_formula_weight         1017.03
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-02-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-09 deposited with the CCDC.	2024-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                76.6020(10)
_cell_angle_beta                 83.3960(10)
_cell_angle_gamma                67.3580(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1913(4)
_cell_length_b                   13.9843(6)
_cell_length_c                   17.7609(8)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.404
_cell_measurement_theta_min      2.183
_cell_volume                     2494.54(18)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2021)'
_computing_data_collection       'APEX3 v2022.10-0 (Bruker, 2022)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon III area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            120957
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.384
_diffrn_reflns_theta_min         2.033
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.2326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0769 before and 0.0535 after correction.
The Ratio of minimum to maximum transmission is 0.8939.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene, pentane'
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10186
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0421P)^2^+2.0222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7751
_reflns_number_total             10186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03364g2.cif
_cod_data_source_block           Thomas_JM-142
_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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1572433--1572439.cif.
;
_cod_original_cell_volume        2494.55(18)
_cod_database_code               1572437
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.932
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(K1) = Uanis(K1B)
3. Rigid body (RIGU) restrains
 O1, O2, C39, C39B, C40, C40B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C39B)=Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(1)
 Sof(K1B)=1-FVAR(2)
 Sof(K1)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C39B(H39C,H39D), C40(H40A,H40B), C40B(H40C,H40D), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C1S(H1S), C2S(H2S),
  C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
;
_shelx_res_checksum              39328
_shelx_hkl_checksum              18437
_olex2_submission_special_instructions 'No special instructions were received'