A new cobalt(ii)–lithium(i) carboxylate complex with an N,O-donor mono-iminoacenaphthenone ligand: synthesis, structure and magnetic behavior
Yambulatov, Dmitriy S.; Nikolaevskii, Stanislav A.; Lukoyanov, Anton N.; Shmelev, Maxim A.; Voronina, Julia K.; Babeshkin, Konstantin A.; Matiukhina, Anna K.; Efimov, Nikolay N.; Kiskin, Mikhail A.; Eremenko, Igor L.; New Journal of Chemistry 47 (2023) 19362–19366; doi:10.1039/D3NJ04144A

data_7062783
_publ_section_title
;
 A new cobalt(ii)--lithium(i) carboxylate complex with an N,O-donor
 mono-iminoacenaphthenone ligand: synthesis, structure and magnetic
 behavior
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19362
_journal_page_last               19366
_journal_paper_doi               10.1039/D3NJ04144A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C68 H80 Co2 Li2 N2 O16, C2 H3 N'
_chemical_formula_sum            'C70 H83 Co2 Li2 N3 O16'
_chemical_formula_weight         1354.13
_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
_audit_creation_date             2023-01-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.367(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6202(11)
_cell_length_b                   19.455(2)
_cell_length_c                   16.1507(18)
_cell_measurement_reflns_used    3625
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      29.93
_cell_measurement_theta_min      2.24
_cell_volume                     3579.6(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1497
_diffrn_reflns_av_unetI/netI     0.1879
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46003
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.986
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.3812
_exptl_absorpt_correction_T_min  0.3213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0903 before and 0.0810 after correction.
The Ratio of minimum to maximum transmission is 0.8429.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 1874 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(19)
_refine_ls_extinction_coef       0.026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     879
_refine_ls_number_reflns         12260
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1644
_refine_ls_R_factor_gt           0.0840
_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^)+(0.1003P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.2137
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                6545
_reflns_number_total             12260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04144a2.cif
_cod_data_source_block           a_a
_cod_depositor_comments          'Adding full bibliography for 7062783.cif.'
_cod_original_cell_volume        3579.6(7)
_cod_database_code               7062783
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.954
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1(10)
 0(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C2S'-N1S'
 1.01 with sigma of 0.02
 C1S'-C2S'
 1.45 with sigma of 0.02
 C1S'-N1S'
 2.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N1S) \\sim Ueq, Uanis(C2S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C10') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1S') \\sim Ueq, Uanis(C2S') \\sim Ueq, Uanis(N1S') \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C9') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8') = Uanis(C8)
Uanis(N1S') = Uanis(N1S)
Uanis(C9) = Uanis(C9')
Uanis(C2S) = Uanis(C2S')
Uanis(C1A) = Uanis(C10')
Uanis(C23) = Uanis(C24)
Uanis(C1S') = Uanis(C1S)
5. Others
 Sof(C10')=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C8')=Sof(H8'A)=Sof(H8'B)=
 Sof(H8'C)=Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(H9'C)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
 Sof(C1S')=Sof(H1SD)=Sof(H1SE)=Sof(H1SF)=Sof(C2S')=Sof(N1S')=1-FVAR(2)
 Sof(N1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C35(H35), C36(H36), C39(H39), C40(H40), C42(H42),
 C43(H43), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C60(H60),
  C61(H61), C62(H62), C64(H64), C65(H65), C66(H66)
6.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10'(H10A,H10B,H10C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C37(H37A,
 H37B,H37C), C44(H44A,H44B,H44C), C1S(H1SA,H1SB,H1SC), C8'(H8'A,H8'B,H8'C),
 C9'(H9'A,H9'B,H9'C), C1A(H1AA,H1AB,H1AC), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C24(H24A,H24B,H24C), C1S'(H1SD,H1SE,H1SF)
;
_shelx_res_checksum              87042
_olex2_submission_special_instructions 'No special instructions were received'