One-pot synthesis of functionalized 4-hydroxy-3-thiomethylcoumarins: Detection and discrimination of Co2+ and Ni2+ ions
Khan, Abu Taleb; Dar, Ajaz Ahmad; Hussain, Sameer; Dutta, Debasish; Iyer, Parameswar K.; RSC Adv.  (2015) –; doi:10.1039/C5RA09152G

data_7220892
_publ_section_title
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 One-pot synthesis of functionalized 4-hydroxy-3-thiomethylcoumarins:
 Detection and discrimination of Co2+ and Ni2+ ions
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA09152G
_journal_year                    2015
_chemical_formula_moiety         'C34 H28 Co N2 O6 S2, 2(C H2 Cl2)'
_chemical_formula_sum            'C36 H32 Cl4 Co N2 O6 S2'
_chemical_formula_weight         853.49
_chemical_name_systematic        'AD_DD_21_Co Complex'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-11 deposited with the CCDC.
2015-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                82.838(5)
_cell_angle_beta                 69.409(4)
_cell_angle_gamma                73.262(4)
_cell_formula_units_Z            1
_cell_length_a                   8.3365(6)
_cell_length_b                   11.1277(8)
_cell_length_c                   11.2945(8)
_cell_measurement_temperature    296(2)
_cell_volume                     938.94(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13358
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             437
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/Methanol'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1553
_reflns_number_gt                2655
_reflns_number_total             3333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra09152g2.cif
_cod_data_source_block           ajaz2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               7220892