Conversion of hydrazides into N,N'-diacylhydrazines in the presence of ruthenium(II)-arene complex
Nikolić, Stefan; Ćirić, Ivanka; Roller, Alexander; Lukes, Vladimir; Arion, Vladimir; Grguric-Sipka, Sanja; New J. Chem. 41 (2017) 6857–6865; doi:10.1039/C7NJ00965H

data_7056276
_publ_section_title
;
 Conversion of hydrazides into N,N'-diacylhydrazines in the presence of
 ruthenium(II)-arene complex
;
_journal_issue                   14
_journal_name_full               'New J. Chem.'
_journal_page_first              6857
_journal_page_last               6865
_journal_paper_doi               10.1039/C7NJ00965H
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety
'0.5(C13 H22 N2 O Ru), 1.5(Cl), 0.5(C13 H22 Cl N2 O Ru)'
_chemical_formula_sum            'C13 H22 Cl2 N2 O Ru'
_chemical_formula_weight         394.29
_chemical_name_systematic
;
[RuCl(propionylhydrazine)(?6-p-cymene)]Cl
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-12 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.2769(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.8233(6)
_cell_length_b                   20.4127(9)
_cell_length_c                   12.0459(5)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.26
_cell_volume                     3308.2(2)
_computing_cell_refinement       'APEX2 v2013.6-2'
_computing_data_collection       'APEX2 v2013.6-2'
_computing_data_reduction        'APEX2 v2013.6-2'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1638
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            73955
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.813
_diffrn_source                   'INCOATEC microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0903 before and 0.0523 after correction. 
The Ratio of minimum to maximum transmission is 0.9300. 
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6072
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0428P)^2^+0.0437P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5347
_reflns_number_total             6072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00965h2.cif
_cod_data_source_block           sagrpah_p21c
_cod_database_code               7056276
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.705
_shelx_res_checksum              24873