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_7063487
_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, C16 H36 N'
_chemical_formula_sum            'C33 H46 Cl3 N4 O Rh'
_chemical_formula_weight         724.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-08-08 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.0387(18)
_cell_length_b                   10.4088(6)
_cell_length_c                   11.1178(5)
_cell_measurement_reflns_used    5493
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.8733
_cell_measurement_theta_min      2.3072
_cell_volume                     3360.4(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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
Data collection was performed by Taisiya S. Sukhikh 
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  0.0990
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46466
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.744
_diffrn_reflns_theta_min         2.307
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6262
_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 0.1024  before and 0.0759  after correction.
 The Ratio of minimum to maximum transmission is 0.8396. 
Additional spherical absorption correction applied with mu*r =  0.2000
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 2510 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         8528
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                6517
_reflns_number_total             8528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03595j2.cif
_cod_data_source_block           IB144
_cod_depositor_comments
'Adding full bibliography for 7063486--7063487.cif.'
_cod_database_code               7063487
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              96352