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_7220891
_publ_section_title
;
 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 N2 Ni O6 S2'
_chemical_formula_sum            'C34 H28 N2 Ni O6 S2'
_chemical_formula_weight         683.41
_chemical_name_systematic        'AD_DD_21_Ni 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                76.635(17)
_cell_angle_beta                 83.429(17)
_cell_angle_gamma                72.903(17)
_cell_formula_units_Z            2
_cell_length_a                   8.1460(16)
_cell_length_b                   11.425(2)
_cell_length_c                   17.576(4)
_cell_measurement_reflns_used    1130
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.0710
_cell_measurement_theta_min      2.9261
_cell_volume                     1519.2(6)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1085
_diffrn_reflns_av_sigmaI/netI    0.2062
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10908
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Face indexing'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             708
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/Methanol'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.2339
_refine_ls_R_factor_gt           0.1013
_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^)+(0.0000P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.2041
_reflns_number_gt                3126
_reflns_number_total             5482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra09152g2.cif
_cod_data_source_block           exp_1982
_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_original_cell_volume        1519.3(5)
_cod_database_code               7220891