Ruthenium(III) complex derived from N,N´-bis(salicylidene)ethylenediamine as chemosensor for the selective recognition of acetate and its interaction with cells for bio-imaging: Experimental and theoretical studies
Pandiyan, T.; Hernandez, Jose Hernandez; Huerta Aguilar, Carlos Alberto; Höpfl, Herbert; New J. Chem. 41 (2017) 10815–10827; doi:10.1039/C7NJ01591G

data_7056512
_publ_section_title
;
 Ruthenium(III) complex derived from
 N,N&#x00B4;-bis(salicylidene)ethylenediamine as chemosensor for the
 selective recognition of acetate and its interaction with cells for
 bio-imaging: Experimental and theoretical studies
;
_journal_issue                   19
_journal_name_full               'New J. Chem.'
_journal_page_first              10815
_journal_page_last               10827
_journal_paper_doi               10.1039/C7NJ01591G
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         '2(C34 H31 N2 O3 P Ru), 2(F6 P), C H2 Cl2'
_chemical_formula_sum            'C69 H64 Cl2 F12 N4 O6 P4 Ru2'
_chemical_formula_weight         1670.16
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-04-27 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                67.616(4)
_cell_angle_beta                 73.070(3)
_cell_angle_gamma                70.037(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7679(2)
_cell_length_b                   13.1943(5)
_cell_length_c                   15.3233(6)
_cell_measurement_reflns_used    13359
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8670
_cell_measurement_theta_min      3.2560
_cell_volume                     1686.57(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    4.00   77.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000  -60.0000 73

  2 omega   -8.00   83.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -       15.2374   77.0000 -180.0000 91

  3 omega   -6.00   83.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -       15.2374   77.0000   60.0000 89

  4 omega  -28.00   41.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -19.0000   60.0000 69

  5 omega  -51.00   40.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -77.0000  -60.0000 91

  6 omega  -45.00   32.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -57.0000 -180.0000 77

  7 omega  -56.00   -3.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -      -16.1749  -57.0000  -60.0000 53

  8 omega  -52.00   32.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -57.0000   30.0000 84

  9 omega  -66.00  -31.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -      -16.1749  118.0000   49.5507 35

 10 omega  -74.00  -42.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -      -16.1749  133.0000  128.9445 32

 11 omega  -73.00  -41.00   1.0000   12.1900
omega____ theta____ kappa____ phi______ frames
    -      -16.1749  131.0000 -108.4611 32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0271946000
_diffrn_orient_matrix_UB_12      -0.0293684000
_diffrn_orient_matrix_UB_13      -0.0344444000
_diffrn_orient_matrix_UB_21      0.0011533000
_diffrn_orient_matrix_UB_22      -0.0523273000
_diffrn_orient_matrix_UB_23      0.0374806000
_diffrn_orient_matrix_UB_31      -0.0737604000
_diffrn_orient_matrix_UB_32      0.0050825000
_diffrn_orient_matrix_UB_33      -0.0020416000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.591
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       prism
_exptl_crystal_F_000             844
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.233
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         5930
_refine_ls_number_restraints     642
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+15.6450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.1813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5664
_reflns_number_total             5930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01591g2.cif
_cod_data_source_block           rutenio
_cod_original_cell_volume        1686.56(12)
_cod_database_code               7056512
_chemical_oxdiff_formula         'C H N O F Cl P Ru'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C41-Cl1 = C41-Cl2
 1.75 with sigma of 0.01
3. Rigid bond restraints
 P2A, F1A, F2A, F3A, F4A, F5A, F6A, P2B, F1B, F2B, F3B, F4B, F5B, F6B, P2C,
 F1C, F2C, F3C, F4C, F5C, F6C
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C41, Cl1, Cl2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
P2A \\sim F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A \\sim P2B \\sim
F1B \\sim F2B \\sim F3B \\sim F4B \\sim F5B \\sim F6B \\sim P2C \\sim F1C \\sim
F2C \\sim F3C \\sim F4C \\sim F5C \\sim F6C: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C41 \\sim Cl1 \\sim Cl2: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Same fragment restrains
{P2B, F1B, F2B, F3B, F4B, F5B, F6B} sigma for 1-2: 0.02, 1-3: 0.04
{P2C, F1C, F2C, F3C, F4C, F5C, F6C} sigma for 1-2: 0.02, 1-3: 0.04
as
{P2A, F1A, F2A, F3A, F4A, F5A, F6A}
6. Others
 1*[Sof(P2A)+Sof(F1A)+Sof(F2A)+Sof(F3A)+Sof(F4A)+Sof(F5A)+Sof(F6A)]+1*
 [Sof(P2B)+Sof(F1B)+Sof(F2B)+Sof(F3B)+Sof(F4B)+Sof(F5B)+Sof(F6B)]+1*[Sof(P2C)+
 Sof(F1C)+Sof(F2C)+Sof(F3C)+Sof(F4C)+Sof(F5C)+Sof(F6C)]=1 with esd of 0.00001
 Sof(P2A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
 Sof(P2B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=FVAR(2)
 Sof(P2C)=Sof(F1C)=Sof(F2C)=Sof(F3C)=Sof(F4C)=Sof(F5C)=Sof(F6C)=FVAR(3)
 Fixed Sof: C41(0.5) H41A(0.5) H41B(0.5) Cl1(0.5) Cl2(0.5)
7.a Rotating group:
 O3(H3A,H3B)
7.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C41(H41A,H41B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34)
;
_shelx_res_checksum              65441
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'