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_1572439
_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         'C38 H32 Co N2 P2, C12 H24 K O6, 4(C6 H6)'
_chemical_formula_sum            'C74 H80 Co K N2 O6 P2'
_chemical_formula_weight         1253.37
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-02-19
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.2827(5)
_cell_length_b                   24.3783(12)
_cell_length_c                   46.956(2)
_cell_measurement_reflns_used    9377
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.219
_cell_measurement_theta_min      2.409
_cell_volume                     12915.4(10)
_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 0.998
_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  0.0533
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            292204
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_min         1.989
_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    0.435
_exptl_absorpt_correction_T_max  0.0452
_exptl_absorpt_correction_T_min  0.0248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1249 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.5487.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             5296
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene, pentane'
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.492(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1514
_refine_ls_number_reflns         26444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0636P)^2^+5.6899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                23207
_reflns_number_total             26444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03364g2.cif
_cod_data_source_block           Thomas_JM-117
_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        12915.5(11)
_cod_database_code               1572439
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.508(12)
 0.492(12)
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:
 C7(H7A,H7B), C8(H8A,H8B), C45(H45A,H45B), C46(H46A,H46B), C77(H77A,H77B),
 C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B),
  C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,
 H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B),
 C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B),
  C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), 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), C41(H41), C42(H42), C43(H43),
  C44(H44), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55),
 C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64),
  C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72), C73(H73),
 C74(H74), C75(H75), C76(H76), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S),
  C6S(H6S), C7S(H7S), C8S(H8S), C9S(H9S), C10S(H10S), C11S(H11S), C12S(H12S),
 C13S(H13S), C14S(H14S), C15S(H15S), C16S(H16S), C17S(H17S), C18S(H18S),
 C19S(H19S), C20S(H20S), C21S(H21S), C22S(H22S), C23S(H23S), C24S(H24S),
 C25S(H25S), C26S(H26S), C27S(H27S), C28S(H28S), C29S(H29S), C30S(H30S),
 C31S(H31S), C32S(H32S), C33S(H33S), C34S(H34S), C35S(H35S), C36S(H36S),
 C37S(H37S), C38S(H38S), C39S(H39S), C40S(H40S), C41S(H41S), C42S(H42S),
 C43S(H43S), C44S(H44S), C45S(H45S), C46S(H46S), C47S(H47S), C48S(H48S)
3.c Fitted hexagon refined as free rotating group:
 C1S(C2S,C3S,C4S,C5S,C6S), C7S(C8S,C9S,C10S,C11S,C12S), C19S(C20S,C21S,C22S,
 C23S,C24S)
;
_shelx_res_checksum              88257
_shelx_hkl_checksum              44008
_olex2_submission_special_instructions 'No special instructions were received'