Di-ruthenium complexes of 1,4-diazabutadiene ligands: synthesis, characterization and utilization as catalyst precursors for the oxidative coupling of amines to imines in air
Saha, Rumpa; Mukherjee, Aparajita; Bhattacharya, Samaresh; New Journal of Chemistry 47 (2023) 12709–12717; doi:10.1039/D3NJ01030A

data_7062586
_publ_section_title
;
 Di-ruthenium complexes of 1,4-diazabutadiene ligands: synthesis,
 characterization and utilization as catalyst precursors for the oxidative
 coupling of amines to imines in air
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12709
_journal_page_last               12717
_journal_paper_doi               10.1039/D3NJ01030A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C64 H50 Cl7 N4 P2 Ru2, [C7H8,Cl-, 0.7 H2O]'
_chemical_formula_sum            'C71 H59.4 Cl8 N4 O0.7 P2 Ru2'
_chemical_formula_weight         1526.6
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_audit_creation_date             2023-06-05
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-06-08 deposited with the CCDC.	2023-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.647(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.926(5)
_cell_length_b                   17.173(2)
_cell_length_c                   26.459(3)
_cell_measurement_reflns_used    220
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.20
_cell_volume                     13705(3)
_computing_data_collection       'APEX3 (Bruker)'
_computing_data_reduction        'APEX3 (Bruker)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.9939
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1663
_diffrn_reflns_av_unetI/netI     0.1186
_diffrn_reflns_Laue_measured_fraction_full 0.9969
_diffrn_reflns_Laue_measured_fraction_max 0.9939
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            87124
_diffrn_reflns_point_group_measured_fraction_full 0.9969
_diffrn_reflns_point_group_measured_fraction_max 0.9939
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.845
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5584.319
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.1257
_refine_diff_density_min         -1.9612
_refine_diff_density_rms         0.2840
_refine_ls_d_res_high            0.7793
_refine_ls_d_res_low             9.2472
_refine_ls_goodness_of_fit_ref   1.1102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    100
_refine_ls_number_parameters     712
_refine_ls_number_reflns         15065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1102
_refine_ls_R_factor_all          0.1813
_refine_ls_R_factor_gt           0.1066
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1869P)^2^+65.9447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2900
_refine_ls_wR_factor_ref         0.3686
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              38
_reflns_limit_h_min              -42
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                7808
_reflns_number_total             15065
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj01030a2.cif
_cod_data_source_block           SB-RS-26AA
_cod_database_code               7062586
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C112(H112), C1(H1), C8(H8), C2(H2), C14(H14), C126(H126), C27(H27), C10(H10),
 C28(H28), C232(H232), C13(H13), C4(H4), C15(H15), C222(H222), C135(H135),
 C116(H116), C114(H114), C216(H216), C233(H233), C123(H123), C236(H236),
 C133(H133), C25(H25), C21(H21), C212(H212), C234(H234), C19(H19), C18(H18),
 C122(H122), C113(H113), C124(H124), C24(H24), C115(H115), C5(H5), C134(H134),
 C7(H7), C16(H16), C136(H136), C11(H11), C22(H22), C132(H132), C125(H125),
 C226(H226), C223(H223), C213(H213), C224(H224), C214(H214), C225(H225),
 C235(H235), C215(H215)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 600 electrons were 
found in a volume of 2808\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
[+ solvents] per Formula Unit 
which account for 592 electrons 
per unit cell.
;
_olex2_submission_special_instructions 'No special instructions were received'