Selective extraction of Pd(ii) by p-tert-butylcalix[4]arenedicarboxylic acid
Morohashi, N.; Iijima, S.; Akasaka, K.; Hattori, T.; New J. Chem. 41 (2017) 2231–; doi:10.1039/C6NJ03839E

data_7056020
_publ_section_title
;
 Selective extraction of Pd(ii) by p-tert-butylcalix[4]arenedicarboxylic
 acid
;
_journal_issue                   6
_journal_name_full               'New J. Chem.'
_journal_page_first              2231
_journal_paper_doi               10.1039/C6NJ03839E
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C112 H138 N10 O12 Pd2'
_chemical_formula_weight         2029.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-12-01 deposited with the CCDC.
2017-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.0605(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3860(11)
_cell_length_b                   18.8479(17)
_cell_length_c                   22.508(2)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.23
_cell_volume                     5234.0(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29550
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6479
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.165
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         11879
_refine_ls_number_restraints     1214
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+10.7244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                9840
_reflns_number_total             11879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj03839e2.cif
_cod_data_source_block           PdComplex
_cod_depositor_comments          'Adding full bibliography for 7056020.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7056020