Rhodium complexes bearing 2-(pyridin-2-yl)hydrazino acenaphthene-1-one: synthesis, structure and electrochemical studies
Bakaev, I. V.; Komlyagina, V. I.; Ulantikov, A. A.; Romashev, N. F.; Gushchin, A. L.; New Journal of Chemistry 48 (2024) 18456–18464; doi:10.1039/D4NJ03595J

data_7063486
_publ_section_title
;
 Rhodium complexes bearing 2-(pyridin-2-yl)hydrazino acenaphthene-1-one:
 synthesis, structure and electrochemical studies
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18456
_journal_page_last               18464
_journal_paper_doi               10.1039/D4NJ03595J
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C17 H10 Cl3 N3 O Rh, C17 H12 N3 O, C3 H6 O'
_chemical_formula_sum            'C37 H28 Cl3 N6 O3 Rh'
_chemical_formula_weight         813.91
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-09-25 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                102.111(4)
_cell_angle_beta                 95.984(4)
_cell_angle_gamma                102.789(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8222(10)
_cell_length_b                   13.4017(15)
_cell_length_c                   15.0898(18)
_cell_measurement_reflns_used    2701
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.0002
_cell_measurement_theta_min      2.7963
_cell_volume                     1679.7(3)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2016)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
Data collection was performed by Danil V. Kochelakov 
in XRD Facility of NIIC SB RAS.
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0919
_diffrn_reflns_Laue_measured_fraction_full 0.995
_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       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19739
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         2.368
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
wR2(int) was 0.0973 before and 0.0564 after correction.
 The Ratio of minimum to maximum transmission is 0.8277. 
Additional spherical absorption correction applied with mu*r =  0.2000
;
_exptl_crystal_colour            'clear yellowish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/diethyl either'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0453P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5216
_reflns_number_total             7675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03595j2.cif
_cod_data_source_block           IB83
_cod_depositor_comments
'Adding full bibliography for 7063486--7063487.cif.'
_cod_database_code               7063486
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              88375