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_1572433
_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_absolute_configuration ad
_chemical_formula_moiety         'C42 H38 Co N2 O P2, F6 P, C4 H8 O'
_chemical_formula_sum            'C46 H46 Co F6 N2 O2 P3'
_chemical_formula_weight         924.69
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                90
_cell_angle_beta                 96.740(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8969(4)
_cell_length_b                   13.5727(5)
_cell_length_c                   14.1536(6)
_cell_measurement_reflns_used    5480
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.308
_cell_measurement_theta_min      2.236
_cell_volume                     2078.86(14)
_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 0.996
_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  0.0847
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            137217
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.412
_diffrn_reflns_theta_min         1.882
_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    0.598
_exptl_absorpt_correction_T_max  0.093181
_exptl_absorpt_correction_T_min  0.060819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1191 before and 0.0609 after correction.
 
For component 2:
 wR2(int) was 0.1357 before and 0.0706 after correction.
 The Ratio of minimum to maximum transmission is 0.66.

Final HKLF 4 output contains 137217 reflections, Rint = 0.0847
 (83935 with I > 3sig(I), Rint = 0.0714)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, diethyl ether'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 3509 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8507
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0468P)^2^+0.6284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7894
_reflns_number_total             8507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03364g2.cif
_cod_data_source_block           Thomas_JM-166
_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_database_code               1572433
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.625(3)
 0.375(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,
 H5SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB), C8S(H8SA,H8SB)
3.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), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              93623
_shelx_hkl_checksum              15720
_olex2_submission_special_instructions 'No special instructions were received'