Toxic heavy metal ‒ Pb, Cd, Sn ‒ complexation by the octadentate hydroxypyridinonate ligand archetype 3,4,3-LI(1,2-HOPO)
Deblonde, Gauthier J.-P.; Lohrey, Trevor D.; An, Dahlia D.; Abergel, Rebecca J.; New Journal of Chemistry 42 (2018) 7649–; doi:10.1039/C7NJ04559J

data_7056969
_publ_section_title
;
 Toxic heavy metal -- Pb, Cd, Sn -- complexation by the octadentate
 hydroxypyridinonate ligand archetype 3,4,3-LI(1,2-HOPO)
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7649
_journal_paper_doi               10.1039/C7NJ04559J
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         '(C34 H34 N8 O12 Sn), 3(H2 O)'
_chemical_formula_sum            'C34 H40 N8 O15 Sn'
_chemical_formula_weight         919.42
_chemical_name_common            'Sn(1,2-HOPO) trihydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-20 deposited with the CCDC.
2018-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0345(7)
_cell_length_b                   17.0024(7)
_cell_length_c                   13.3898(6)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.22
_cell_measurement_theta_min      2.61
_cell_volume                     3650.4(3)
_computing_cell_refinement       'SAINT V8.37A Bruker, Madison, WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison, WI'
_computing_data_reduction        'SAINT V8.37A Bruker, Madison, WI'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 Bruker, Madison, WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'phi and omega shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31453
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         40.220
_diffrn_reflns_theta_min         2.525
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       shard
_exptl_crystal_F_000             1880
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.680
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 3278 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         8824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.8315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                7861
_reflns_number_total             8824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04559j2.cif
_cod_data_source_block           SnHOPO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7056969.cif.
;
_cod_database_code               7056969
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              13312