Effect of coordinating (–CN) vs. non-coordinating (–F) substituents in 3-pyridyl urea receptors toward second sphere sulfate recognition: selective crystallisation of CuSO4 from mixtures of competing anions/cations
Akhuli, Bidyut; Ghosh, Tamal Kanti; Ghosh, Pradyut; CrystEngComm 15 (2013) 9472–; doi:10.1039/c3ce40974k

data_7210928
_publ_section_title
;
 Effect of coordinating (--CN) vs. non-coordinating (--F) substituents in
 3-pyridyl urea receptors toward second sphere sulfate recognition:
 selective crystallisation of CuSO4 from mixtures of competing
 anions/cations
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9472
_journal_paper_doi               10.1039/c3ce40974k
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C52 H40 Cu N16 O8 S'
_chemical_formula_weight         1112.60
_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
_cell_angle_alpha                98.663(2)
_cell_angle_beta                 109.9000(10)
_cell_angle_gamma                103.784(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2254(8)
_cell_length_b                   14.6731(9)
_cell_length_c                   17.1748(10)
_cell_measurement_reflns_used    8525
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.59
_cell_measurement_theta_min      2.39
_cell_volume                     2944.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'MERCURY 3.1'
_computing_publication_material  'ORTEP 3v.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0543
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43020
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.9634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1146
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
The unit cell contains some disordered solvent molecules which has been treated as a diffuse contribution to the overall scatterin without
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.422
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         10556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+2.8182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1522
_reflns_number_gt                8144
_reflns_number_total             10556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40974k.txt
_cod_data_source_block           PY4CNU_CuSO4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7210928