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_7062587
_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         'C68 H62 Cl3 N4 P2 Ru2, [C7H8,  Cl-, H2O]'
_chemical_formula_sum            'C75 H72 Cl4 N4 O P2 Ru2'
_chemical_formula_weight         1450.188
_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                 112.892(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.5574(15)
_cell_length_b                   17.2458(6)
_cell_length_c                   26.4277(10)
_cell_measurement_reflns_used    195
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      1.36
_cell_volume                     13669.9(10)
_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)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.9942
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.9969
_diffrn_reflns_Laue_measured_fraction_max 0.9942
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            114130
_diffrn_reflns_point_group_measured_fraction_full 0.9969
_diffrn_reflns_point_group_measured_fraction_max 0.9942
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.687
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5548.932
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.9623
_refine_diff_density_min         -1.0482
_refine_diff_density_rms         0.1029
_refine_ls_d_res_high            0.7659
_refine_ls_d_res_low             14.9966
_refine_ls_goodness_of_fit_ref   1.1085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     778
_refine_ls_number_reflns         15848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1085
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0423P)^2^+21.7771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              39
_reflns_limit_h_min              -42
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                11833
_reflns_number_total             15848
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj01030a2.cif
_cod_data_source_block           SB-RS-21F
_cod_original_formula_sum        'C75 H72 Cl4 N4 O1 P2 Ru2'
_cod_database_code               7062587
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C20(H20), C21(H21), C23(H23), C24(H24), C17(H17), C18(H18),
 C31(H31), C30(H30), C28(H28), C27(H27), C226(H226), C225(H225), C224(H224),
 C223(H223), C222(H222), C232(H232), C233(H233), C234(H234), C235(H235),
 C236(H236), C212(H212), C213(H213), C214(H214), C215(H215), C216(H216),
 C15(H15), C14(H14), C12(H12), C11(H11), C4(H4), C5(H5), C7(H7), C8(H8),
 C136(H136), C135(H135), C134(H134), C133(H133), C132(H132), C126(H126),
 C125(H125), C124(H124), C123(H123), C122(H122), C112(H112), C113(H113),
 C114(H114), C115(H115), C116(H116)
1.b Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C25(H25a,H25b,H25c), C32(H32a,H32b,H32c), C33(H33a,H33b,
 H33c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 616 electrons were 
found in a volume of 2804\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
[+ solvents] per Formula Unit 
which account for 616 electrons 
per unit cell.
;
_olex2_submission_special_instructions 'No special instructions were received'