Rhodamine-azo based two fluorescent probes for recognition of trivalent metal ions: crystal structures elucidation and biological application
Mandal, Jayanta; Pal, Kunal; Ghosh Chowdhury, Sougata; Karmakar, Parimal; Panja, Anangamohan; Banerjee, Snehasis; Saha, Amrita; Dalton Transactions  (2022) –; doi:10.1039/D2DT00399F

data_7711225
_publ_section_title
;
 Rhodamine-azo based two fluorescent probes for recognition of trivalent
 metal ions: crystal structures elucidation and biological application
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00399F
_journal_year                    2022
_chemical_formula_moiety         'C40 H36 N6 O4, C H Cl3'
_chemical_formula_sum            'C41 H37 Cl3 N6 O4'
_chemical_formula_weight         784.11
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-06 deposited with the CCDC.	2022-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.173(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1315(19)
_cell_length_b                   11.7069(10)
_cell_length_c                   17.5826(15)
_cell_measurement_reflns_used    4996
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.110
_cell_measurement_theta_min      1.976
_cell_volume                     4469.3(7)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Mercury (Macrae et al 2008)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1026
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            152821
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.110
_diffrn_reflns_theta_min         1.976
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.984
_exptl_transmission_factor_min   0.782
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         9820
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1512P)^2^+1.9601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2458
_refine_ls_wR_factor_ref         0.2998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4989
_reflns_number_total             9820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00399f2.cif
_cod_data_source_block           HL1
_cod_database_code               7711225
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Cl3A \\sim Cl2 \\sim Cl2A \\sim Cl12 \\sim Cl1A \\sim Cl3 \\sim C43: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
3. Others
 Fixed Sof: C101(0.7) H10A(0.7) H10B(0.7) H10C(0.7) Cl2(0.75) Cl3(0.75)
 Cl12(0.75) Cl2A(0.25) Cl1A(0.25) Cl3A(0.25) C13(0.3) H13A(0.3) H13B(0.3)
 H13C(0.3)
4.a Ternary CH refined with riding coordinates:
 C43(H43)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
4.c Me refined with riding coordinates:
 C101(H10A,H10B,H10C)
4.d Aromatic/amide H refined with riding coordinates:
 N1(H1), C6(H6), C9(H9), C11(H11), C15(H15), C16(H16), C17(H17), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C33(H33), N2(H2),
 C39(H39), C41(H41)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C38(H38A,H38B,
 H38C), C13(H13A,H13B,H13C)
4.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76537
_shelx_hkl_checksum              82296
_shelx_fab_checksum              72523
_olex2_submission_special_instructions 'No special instructions were received'