Synthesis of a potassium capped terminal cobalt-oxido complex.
Anferov, Sophie W.; Krupinski, Alexandra; Anderson, John S.; Chemical communications (Cambridge, England) 60 (2024) 9562–9565; doi:10.1039/d4cc03014a

data_7133478
_publ_section_title
;
 Synthesis of a potassium capped terminal cobalt-oxido complex.
;
_journal_issue                   71
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9562
_journal_page_last               9565
_journal_paper_doi               10.1039/d4cc03014a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C28 H34 Co K N5 O'
_chemical_formula_sum            'C28 H34 Co K N5 O'
_chemical_formula_weight         554.63
_chemical_name_systematic        '[[tBu,TolDHP]CoOK]2'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-06-19 deposited with the CCDC.	2024-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                89.533(19)
_cell_angle_beta                 73.197(17)
_cell_angle_gamma                64.696(15)
_cell_formula_units_Z            2
_cell_length_a                   10.153(7)
_cell_length_b                   11.686(8)
_cell_length_c                   13.651(10)
_cell_measurement_reflns_used    1128
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      2.28
_cell_volume                     1389.2(17)
_computing_cell_refinement       'APEX4, v.2021.4-0 (Bruker AXS Inc., 2021)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'APEX4, v.2021.4-0 (Bruker AXS Inc., 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2607
_diffrn_reflns_av_unetI/netI     0.2678
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14083
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        23.459
_diffrn_reflns_theta_max         23.459
_diffrn_reflns_theta_min         2.283
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'INCOATEC ImuS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.4624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1297 before and 0.0892 after correction.
The Ratio of minimum to maximum transmission is 0.6210.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       needle
_exptl_crystal_F_000             582
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: petroleum ether'
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.758
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4025
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.2880
_refine_ls_R_factor_gt           0.1435
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3264
_refine_ls_wR_factor_ref         0.4058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1757
_reflns_number_total             4025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03014a3.cif
_cod_data_source_block           0998_sw_jsa1
_cod_depositor_comments
'Adding full bibliography for 7133478--7133479.cif.'
_cod_original_cell_volume        1389.1(17)
_cod_database_code               7133478
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.831
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C00Z) \\sim Ueq, Uanis(C00I) \\sim Ueq, Uanis(N007) \\sim Ueq,
Uanis(C00L) \\sim Ueq, Uanis(C00U) \\sim Ueq, Uanis(C00A) \\sim Ueq,
Uanis(C00B) \\sim Ueq, Uanis(C00W) \\sim Ueq, Uanis(C00H) \\sim Ueq,
Uanis(C00V) \\sim Ueq, Uanis(O003) \\sim Ueq, Uanis(K002) \\sim Ueq,
Uanis(C00S) \\sim Ueq, Uanis(Co01) \\sim Ueq, Uanis(N006) \\sim Ueq,
Uanis(C00Q) \\sim Ueq, Uanis(C00T) \\sim Ueq, Uanis(C00O) \\sim Ueq,
Uanis(C00N) \\sim Ueq, Uanis(C00G) \\sim Ueq, Uanis(C00K) \\sim Ueq,
Uanis(C00P) \\sim Ueq, Uanis(C00R) \\sim Ueq, Uanis(C00J) \\sim Ueq,
Uanis(C00M) \\sim Ueq, Uanis(C00D) \\sim Ueq, Uanis(C00X) \\sim Ueq,
Uanis(C00Y) \\sim Ueq, Uanis(C009) \\sim Ueq, Uanis(C00F) \\sim Ueq,
Uanis(N005) \\sim Ueq, Uanis(N004) \\sim Ueq, Uanis(N008) \\sim Ueq,
Uanis(C010) \\sim Ueq, Uanis(C00C) \\sim Ueq, Uanis(C00E) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(N008) = Uanis(N006) = Uanis(N005)
Uanis(C009) = Uanis(C00I) = Uanis(C00Q) = Uanis(C00C)
Uanis(C00A) = Uanis(C00E)
Uanis(C00R) = Uanis(C00Y)
Uanis(C00J) = Uanis(C00V) = Uanis(C00N) = Uanis(C00W) = Uanis(C00M) =
Uanis(C00K) = Uanis(C00O)
2.a Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00H(H00H), C00K(H00K), C00L(H00L), C00O(H00O),
 C00P(H00P), C00S(H00S)
2.b Idealised Me refined as rotating group:
 C00N(H00A,H00B,H00C), C00T(H00D,H00E,H00I), C00U(H00N,H00Q,H00R), C00V(H00T,
 H00U,H00V), C00W(H00W,H00X,H00Y), C00X(H00Z,H,HA), C00Z(H00,HB,HC), C010(H01A,
 H01B,H01C)
;
_shelx_res_checksum              83903
_shelx_hkl_checksum              48210
_olex2_submission_special_instructions 'No special instructions were received'