Unusual complexation behaviors of R-BTPs with water molecule and Pd(ii) caused by electronic modulation of substituents on BTP backbone: new insights into palladium separation under the framework of minor actinides’ partitioning
Xu, Lei; Zhang, Anyun; Pu, Ning; Lu, Yanchao; Yang, Hua; Liu, Ziyang; Ji, Yanqin; New Journal of Chemistry 43 (2019) 9052–; doi:10.1039/C9NJ00343F

data_7058382
_publ_section_title
;
 Unusual complexation behaviors of R-BTPs with water molecule and Pd(ii)
 caused by electronic modulation of substituents on BTP backbone: new
 insights into palladium separation under the framework of minor
 actinides&#x2019; partitioning
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9052
_journal_paper_doi               10.1039/C9NJ00343F
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C15 H15 N7, 6(H2 O)'
_chemical_formula_sum            'C15 H27 N7 O6'
_chemical_formula_weight         401.44
_chemical_name_systematic        c1-BTP
_chemical_properties_physical    Heat-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-10-02 deposited with the CCDC.    2019-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.817(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3819(15)
_cell_length_b                   6.8739(5)
_cell_length_c                   20.2230(18)
_cell_measurement_reflns_used    1697
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4637
_cell_measurement_theta_min      3.0788
_cell_volume                     2076.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0362899000
_diffrn_orient_matrix_UB_12      -0.0089901000
_diffrn_orient_matrix_UB_13      0.0158217000
_diffrn_orient_matrix_UB_21      -0.0037930000
_diffrn_orient_matrix_UB_22      0.1027553000
_diffrn_orient_matrix_UB_23      0.0007244000
_diffrn_orient_matrix_UB_31      -0.0304156000
_diffrn_orient_matrix_UB_32      -0.0020502000
_diffrn_orient_matrix_UB_33      -0.0324598000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7862
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.14
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/Ethanol'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3795
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.1885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                2507
_reflns_number_total             3795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9nj00343f2.cif
_cod_data_source_block           141023_c1_btp
_cod_depositor_comments
'Adding full bibliography for 7058380--7058383.cif.'
_cod_database_code               7058382
_chemical_oxdiff_formula         'c10 h10 n2'
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1-H1B
 0.86 with sigma of 0.02
 H1A-O1
 0.86 with sigma of 0.02
 H2A-O2
 0.86 with sigma of 0.02
 O3-H3B
 0.86 with sigma of 0.02
 O2-H2B
 0.86 with sigma of 0.02
 H3A-O3
 0.86 with sigma of 0.02
 O4-H4B
 0.86 with sigma of 0.02
 O4-H4A
 0.86 with sigma of 0.02
 H5B-O5
 0.86 with sigma of 0.02
 O5-H5A
 0.86 with sigma of 0.02
 O6-H6A
 0.86 with sigma of 0.02
 H6B-O6
 0.86 with sigma of 0.02
 H4B-O4
 0.86 with sigma of 0.02
3.a Free rotating group:
 O1(H1A), O5(H5A), O2(H2A,H2B), O3(H3A)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C)
;