Ruthenocycles of benzothiazolyl and pyridyl hydrazones with ancillary PAHs: synthesis, structure, electrochemistry and antimicrobial activity
Dinda, Soumitra; Sultana, Tamanna; Sultana, Suhana; Patra, Sarat Chandra; Mitra, Arup Kumar; Roy, Subhadip; Pramanik, Kausikisankar; Ganguly, Sanjib; New Journal of Chemistry 44 (2020) 11022–11034; doi:10.1039/D0NJ01447H

data_7059676
_publ_section_title
;
 Ruthenocycles of benzothiazolyl and pyridyl hydrazones with ancillary
 PAHs: synthesis, structure, electrochemistry and antimicrobial activity
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11022
_journal_page_last               11034
_journal_paper_doi               10.1039/D0NJ01447H
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C55 H42 Cl N3 O P2 Ru S, 1[CH2Cl2]'
_chemical_formula_sum            'C56 H44 Cl3 N3 O P2 Ru S'
_chemical_formula_weight         1076.429
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2020-04-14
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.03.26 svn.re84ffbc8 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-04-19 deposited with the CCDC.	2020-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                78.061(2)
_cell_angle_beta                 78.123(2)
_cell_angle_gamma                67.430(2)
_cell_formula_units_Z            4
_cell_length_a                   12.5638(7)
_cell_length_b                   14.5528(8)
_cell_length_c                   30.3087(16)
_cell_measurement_reflns_used    2482
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.556
_cell_measurement_theta_min      2.399
_cell_volume                     4957.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.14
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9965
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.9978
_diffrn_reflns_Laue_measured_fraction_max 0.9965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            76899
_diffrn_reflns_point_group_measured_fraction_full 0.9978
_diffrn_reflns_point_group_measured_fraction_max 0.9965
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_process_details   'sadabs(sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       prism
_exptl_crystal_F_000             2198.828
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.8304
_refine_diff_density_min         -0.7581
_refine_diff_density_rms         0.1201
_refine_ls_d_res_high            0.7682
_refine_ls_d_res_low             8.3505
_refine_ls_goodness_of_fit_ref   1.0477
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    168
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         22825
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.0476
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+5.2396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                16207
_reflns_number_total             22825
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0nj01447h2.cif
_cod_data_source_block           4b
_cod_depositor_comments
;Adding full bibliography for 7059673--7059676.cif.

 Adding full bibliography for 7059673--7059676.cif.
;
_cod_original_formula_sum        'C56 Cl3 H44 N3 O1 P2 Ru1 S1 '
_cod_database_code               7059676
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C74-O2
 1.32 with sigma of 0.02
 Ru2-Cl2 \\sim Ru2-ClL
 with sigma of 0.001
 O10-C113 \\sim O2-C74
 with sigma of 0.001
3. Others
 Fixed Sof: Cl2(0.5) O2(0.5) C74(0.5) ClL(0.5) C113(0.5) O10(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42),
  C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51),
 C52(H52), C53(H53), C54(H54), C55(H55), C57(H57), C58(H58), C59(H59), C60(H60),
  C63(H63), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71),
 C73(H73), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83),
  C84(H84), C85(H85), C86(H86), C88(H88), C89(H89), C90(H90), C91(H91),
 C92(H92), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98), C100(H100),
 C101(H101), C102(H102), C103(H103), C104(H104), C106(H106), C107(H107),
 C108(H108), C109(H109), C110(H110)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 158 electrons were 
found in a volume of 556\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 1[CH2Cl2] per Formula Unit 
which account for 168 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'