Partial and complete hydrolysis of metal complexes based on monoiminoacenaphthene-1-ones
Lukoyanov, Anton N.; Zvereva, Yulia V.; Cherkasov, Anton V.; Zhigulin, Grigory Yu.; Kharitonov, Nikita P.; Ketkov, Sergey Yu.; CrystEngComm 27 (2025) 1749–1762; doi:10.1039/D4CE01199F

data_7249928
_publ_section_title
;
 Partial and complete hydrolysis of metal complexes based on
 monoiminoacenaphthene-1-ones
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              1749
_journal_page_last               1762
_journal_paper_doi               10.1039/D4CE01199F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C186 H192 Ca3 N6 O6'
_chemical_formula_sum            'C186 H192 Ca3 N6 O6'
_chemical_formula_weight         2727.68
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-10-30 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   26.9692(16)
_cell_length_b                   26.9692(16)
_cell_length_c                   17.5013(11)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.76
_cell_measurement_theta_min      2.49
_cell_volume                     11023.9(12)
_computing_cell_refinement       'Saint 8.37a'
_computing_data_collection       APEX2
_computing_data_reduction        'Saint 8.37a'
_computing_structure_refinement  'SHELXL 2019/2'
_computing_structure_solution    'SHELXT 2018/2'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29412
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.021
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_min         2.097
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       prism
_exptl_crystal_F_000             4374
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL 2019/2'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         4332
_refine_ls_number_restraints     524
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0895
_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^)+(0.1069P)^2^+51.0152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2150
_refine_ls_wR_factor_ref         0.2493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2811
_reflns_number_total             4332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01199f2.cif
_cod_data_source_block           ca3mianh6
_cod_depositor_comments
'Adding full bibliography for 7249926--7249932.cif.'
_cod_original_cell_volume        11023.9(15)
_cod_database_code               7249928
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              59809