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_7134370
_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         'C44 H70 Cl2 Co2 N2 O4 P2'
_chemical_formula_sum            'C44 H70 Cl2 Co2 N2 O4 P2'
_chemical_formula_weight         941.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-10-16
_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                 96.897(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1686(5)
_cell_length_b                   12.4842(6)
_cell_length_c                   18.9809(8)
_cell_measurement_reflns_used    4200
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      24.14
_cell_measurement_theta_min      2.45
_cell_volume                     2392.13(19)
_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      150.0
_diffrn_measured_fraction_theta_full 0.999
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27890
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.394
_diffrn_reflns_theta_min         2.171
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.5819
_exptl_absorpt_correction_T_min  0.4986
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1150 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.8568.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             996
_refine_diff_density_max         2.423
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4391
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0569P)^2^+7.0255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3919
_reflns_number_total             4391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06550f2.cif
_cod_data_source_block           mo_reco_air_0m_a
_cod_depositor_comments
'Adding full bibliography for 7134368--7134372.cif.'
_cod_database_code               7134370
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 C9-C2 \\sim C2-C9A
 with sigma of 0.02
 C10A-C9A \\sim C9-C10
 with sigma of 0.02
3. Rigid bond restraints
 C9A, C10A, C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C9A \\sim C10A \\sim C9 \\sim C10: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C9) = Uanis(C9A)
5. Others
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C7(H7A,H7B), C9A(H9AA,H9AB), C9(H9A,H9B)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C15(H15)
6.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10A(H10A,H10B,H10C),
  C10(H10D,H10E,H10F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64399
_shelx_hkl_checksum              64558
_olex2_submission_special_instructions 'No special instructions were received'