Isolation and oxygen activation of electron-rich CoII4O metallic clusters having a 3-fold symmetry
Francis, Maria; Patra, Asutosh; Salam, Farsana Abdul; Ungur, Liviu; Schwarz, Björn; Roy, Sudipta; Chemical Communications 61 (2025) 6897–6900; doi:10.1039/D4CC06550F

data_7134372
_publ_section_title
;
 Isolation and oxygen activation of electron-rich CoII4O metallic clusters
 having a 3-fold symmetry
;
_journal_issue                   38
_journal_name_full               'Chemical Communications'
_journal_page_first              6897
_journal_page_last               6900
_journal_paper_doi               10.1039/D4CC06550F
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C66 H105 Cl3 Co4 N3 O1 P3'
_chemical_formula_sum            'C66 H105 Cl3 Co4 N3 O P3'
_chemical_formula_weight         1391.50
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-10 deposited with the CCDC.	2025-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   23.4395(6)
_cell_length_b                   23.4395(6)
_cell_length_c                   21.0260(8)
_cell_measurement_reflns_used    9364
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.80
_cell_volume                     10004.2(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            184854
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_min         2.182
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6510
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1166 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.8734.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_F_000             4404
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.131
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.026(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4504
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0143
_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^)+(0.0211P)^2^+6.1301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0368
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                4479
_reflns_number_total             4504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06550f2.cif
_cod_data_source_block           mo_reco_0m_a
_cod_depositor_comments
'Adding full bibliography for 7134368--7134372.cif.'
_cod_original_cell_volume        10004.2(6)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7134372
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.974(8)
 0.026(8)
2. 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
3.a Ternary CH refined with riding coordinates:
 C11(H11), C13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C17(H17A,H17B), C19(H19A,H19B)
3.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C4(H4), C5(H5)
3.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C3(H3A,
 H3B,H3C)
;
_shelx_res_checksum              34464
_shelx_hkl_checksum              58910
_olex2_submission_special_instructions 'No special instructions were received'