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_1572438
_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
'C41 H39 Co N2 P3, 0.784(C4 H8 O), 0.216(C6 H6), F6 P'
_chemical_formula_sum            'C45.44 H46.56 Co F6 N2 O0.79 P4'
_chemical_formula_weight         930.00
_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             2024-07-04
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                87.1280(10)
_cell_angle_beta                 75.067(2)
_cell_angle_gamma                85.5970(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4936(5)
_cell_length_b                   12.2636(5)
_cell_length_c                   15.7199(7)
_cell_measurement_reflns_used    9067
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.420
_cell_measurement_theta_min      2.537
_cell_volume                     2133.56(16)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2021)'
_computing_data_collection       'APEX3 v2021.10-0 (Bruker, 2021)'
_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      100.00
_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 0.993
_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  0.0404
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            96743
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.504
_diffrn_reflns_theta_min         2.480
_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    0.616
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0618 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.7564.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             961
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, C6H6'
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.047
_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     625
_refine_ls_number_reflns         8804
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+1.6297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8142
_reflns_number_total             8804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03364g2.cif
_cod_data_source_block           Thomas_JM-293
_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               1572438
_shelx_shelxl_version_number     2019/1
_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. Rigid body (RIGU) restrains
 C1SC, C2SC, C6SC, C3SC, C5SC, C4SC, C2SB, O1SB, C1SB, C4SB, C3SB, O1S, C1S,
 C4S, C2S, C3S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Same fragment restrains
{O1S, C1S, C2S, C3S, C4S} sigma for 1-2: 0.02, 1-3: 0.02
as in
{O1SB, C1SB, C2SB, C3SB, C4SB}
4. Others
 1*[Sof(O1S)+Sof(C1S)+Sof(H1SA)+Sof(H1SB)+Sof(C2S)+Sof(H2SA)+Sof(H2SB)+
 Sof(C3S)+Sof(H3SA)+Sof(H3SB)+Sof(C4S)+Sof(H4SA)+Sof(H4SB)]+1*[Sof(O1SB)+
 Sof(C1SB)+Sof(H1SC)+Sof(H1SD)+Sof(C2SB)+Sof(H2SC)+Sof(H2SD)+Sof(C3SB)+
 Sof(H3SC)+Sof(H3SD)+Sof(C4SB)+Sof(H4SC)+Sof(H4SD)]+1*[Sof(C1SC)+Sof(H1SE)+
 Sof(C2SC)+Sof(H2SE)+Sof(C3SC)+Sof(H3SE)+Sof(C4SC)+Sof(H4SE)+Sof(C5SC)+
 Sof(H5SC)+Sof(C6SC)+Sof(H6SC)]=1 with esd of 0
 Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=
 Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=FVAR(1)
 Sof(O1SB)=Sof(C1SB)=Sof(H1SC)=Sof(H1SD)=Sof(C2SB)=Sof(H2SC)=Sof(H2SD)=
 Sof(C3SB)=Sof(H3SC)=Sof(H3SD)=Sof(C4SB)=Sof(H4SC)=Sof(H4SD)=FVAR(2)
 Sof(C1SC)=Sof(H1SE)=Sof(C2SC)=Sof(H2SE)=Sof(C3SC)=Sof(H3SE)=Sof(C4SC)=
 Sof(H4SE)=Sof(C5SC)=Sof(H5SC)=Sof(C6SC)=Sof(H6SC)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C1SB(H1SC,
 H1SD), C2SB(H2SC,H2SD), C3SB(H3SC,H3SD), C4SB(H4SC,H4SD)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C1SC(H1SE),
 C2SC(H2SE), C3SC(H3SE), C4SC(H4SE), C5SC(H5SC), C6SC(H6SC)
5.c Fitted hexagon refined as free rotating group:
 C1SC(C2SC,C3SC,C4SC,C5SC,C6SC)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              44640
_shelx_hkl_checksum              6197
_olex2_submission_special_instructions 'No special instructions were received'