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_7058381
_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         'C27 H39 N7, H2 O'
_chemical_formula_sum            'C27 H41 N7 O'
_chemical_formula_weight         479.67
_chemical_name_systematic        subt-BTP
_chemical_properties_physical    Heat-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5131(6)
_cell_length_b                   16.9916(5)
_cell_length_c                   26.0514(10)
_cell_measurement_reflns_used    7648
_cell_measurement_temperature    172.0
_cell_measurement_theta_max      29.5597
_cell_measurement_theta_min      2.8567
_cell_volume                     5981.6(4)
_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      172.0
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -64.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8433  -77.0000  -90.0000 104

  2 omega  -85.00   21.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183  -77.0000    0.0000 106

  3 omega  -48.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183   84.0000  136.0000 85
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0511769000
_diffrn_orient_matrix_UB_12      -0.0031689000
_diffrn_orient_matrix_UB_13      0.0056474000
_diffrn_orient_matrix_UB_21      -0.0114953000
_diffrn_orient_matrix_UB_22      0.0194009000
_diffrn_orient_matrix_UB_23      -0.0233625000
_diffrn_orient_matrix_UB_31      -0.0016633000
_diffrn_orient_matrix_UB_32      -0.0368318000
_diffrn_orient_matrix_UB_33      -0.0127960000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37634
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86160
_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_colour_primary    yellow
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/Ethanol'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         5444
_refine_ls_number_restraints     614
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1156P)^2^+3.0892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1928
_refine_ls_wR_factor_ref         0.2166
_reflns_number_gt                3930
_reflns_number_total             5444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9nj00343f2.cif
_cod_data_source_block           150331_subt_btp
_cod_depositor_comments
'Adding full bibliography for 7058380--7058383.cif.'
_cod_original_cell_volume        5981.7(4)
_cod_database_code               7058381
_chemical_oxdiff_formula         'c10 h10 n2 o8'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{H13, H13A}
2. Others
 Fixed Uiso: H1A(0.063) H1B(0.063) H3(0.053) H4(0.046) H2(0.048) H20(0.09)
 H24(0.073) H13(0.135) H26A(0.083) H26B(0.083) H21A(0.122) H21B(0.122)
 H21C(0.122) H9(0.075) H25A(0.119) H25B(0.119) H25C(0.119) H12A(0.13)
 H12B(0.13) H12C(0.13) H22A(0.113) H22B(0.113) H10A(0.138) H10B(0.138)
 H10C(0.138) H11A(0.083) H11B(0.083) H14A(0.196) H14B(0.196) H14C(0.196)
 H27A(0.163) H27B(0.163) H27C(0.163) H15A(0.149) H15B(0.149) H23A(0.171)
 H23B(0.171) H23C(0.171) H16A(0.222) H16B(0.222) H16C(0.222) H26C(0.098)
 H26D(0.098) H24A(0.09) H27D(0.157) H27E(0.157) H27F(0.157) H25D(0.138)
 H25E(0.138) H25F(0.138) H21D(0.122) H21E(0.122) H21F(0.122) H20A(0.094)
 H22C(0.112) H22D(0.112) H23D(0.15) H23E(0.15) H23F(0.15) H11C(0.084)
 H11D(0.084) H9A(0.075) H10D(0.125) H10E(0.125) H10F(0.125) H12D(0.116)
 H12E(0.116) H12F(0.116) H13A(0.139) H15C(0.151) H15D(0.151) H14D(0.197)
 H14E(0.197) H14F(0.197) H16D(0.215) H16E(0.215) H16F(0.215)
 Fixed X: H1A(0.8826) H1B(0.8021) H3(0.8011) H4(0.7037) H2(0.9144) H20(1.1874)
 H24(1.184) H13(0.5027) H26A(1.1005) H26B(1.1728) H21A(1.0201) H21B(1.0672)
 H21C(0.9821) H9(0.5) H25A(1.2824) H25B(1.3066) H25C(1.2376) H12A(0.3584)
 H12B(0.4407) H12C(0.3693) H22A(1.085) H22B(1.1658) H10A(0.674) H10B(0.5841)
 H10C(0.6482) H11A(0.4413) H11B(0.5143) H14A(0.6736) H14B(0.5926) H14C(0.6586)
 H27A(0.9795) H27B(1.0168) H27C(1.0529) H15A(0.4495) H15B(0.537) H23A(1.2099)
 H23B(1.275) H23C(1.2832) H16A(0.3794) H16B(0.3873) H16C(0.4666) H26C(1.2572)
 H26D(1.1788) H24A(1.1858) H27D(1.2959) H27E(1.3469) H27F(1.2488) H25D(1.0564)
 H25E(1.1392) H25F(1.0442) H21D(1.1365) H21E(1.2092) H21F(1.2332) H20A(1.1555)
 H22C(1.0972) H22D(1.0099) H23D(0.9655) H23E(1.0519) H23F(0.9553) H11C(0.4855)
 H11D(0.5755) H9A(0.4639) H10D(0.444) H10E(0.3573) H10F(0.3834) H12D(0.5804)
 H12E(0.6731) H12F(0.6064) H13A(0.493) H15C(0.6272) H15D(0.5497) H14D(0.42)
 H14E(0.4246) H14F(0.5028) H16D(0.6495) H16E(0.7284) H16F(0.7171)
 Fixed Y: H1A(0.3063) H1B(0.313) H3(-0.0662) H4(0.0199) H2(-0.0133)
 H20(0.0865) H24(0.2161) H13(0.3168) H26A(0.3568) H26B(0.3527) H21A(0.0908)
 H21B(0.0053) H21C(0.0181) H9(0.2017) H25A(0.2157) H25B(0.2918) H25C(0.2994)
 H12A(0.1653) H12B(0.1715) H12C(0.0964) H22A(-0.0342) H22B(-0.047) H10A(0.1464)
 H10B(0.0933) H10C(0.0654) H11A(0.0693) H11B(0.0566) H14A(0.4118) H14B(0.4323)
 H14C(0.3546) H27A(0.2897) H27B(0.3567) H27C(0.2677) H15A(0.4254) H15B(0.4321)
 H23A(0.0362) H23B(-0.0349) H23C(0.0505) H16A(0.3181) H16B(0.3949) H16C(0.3256)
 H26C(0.3288) H26D(0.3367) H24A(0.204) H27D(0.1913) H27E(0.2659) H27F(0.2285)
 H25D(0.3347) H25E(0.3149) H25F(0.2594) H21D(-0.0247) H21E(-0.0404)
 H21F(0.0285) H20A(0.0959) H22C(-0.0244) H22D(-0.0137) H23D(0.1193)
 H23E(0.1091) H23F(0.0548) H11C(0.0633) H11D(0.0543) H9A(0.1984) H10D(0.0737)
 H10E(0.0911) H10F(0.1545) H12D(0.1392) H12E(0.1202) H12F(0.1962) H13A(0.3139)
 H15C(0.4363) H15D(0.4419) H14D(0.3394) H14E(0.4183) H14F(0.4042) H16D(0.3388)
 H16E(0.3373) H16F(0.4143)
 Fixed Z: H1A(0.6478) H1B(0.6151) H3(0.6033) H4(0.5542) H2(0.662) H20(0.7943)
 H24(0.8051) H13(0.4413) H26A(0.7652) H26B(0.8139) H21A(0.8411) H21B(0.8492)
 H21C(0.8073) H9(0.4234) H25A(0.7284) H25B(0.7623) H25C(0.7127) H12A(0.4729)
 H12B(0.5169) H12C(0.5145) H22A(0.7447) H22B(0.79) H10A(0.3907) H10B(0.3707)
 H10C(0.419) H11A(0.4323) H11B(0.4806) H14A(0.4604) H14B(0.4176) H14C(0.4123)
 H27A(0.8076) H27B(0.8462) H27C(0.8536) H15A(0.4712) H15B(0.5122) H23A(0.6886)
 H23B(0.7105) H23C(0.7359) H16A(0.519) H16B(0.5543) H16C(0.5603) H26C(0.7761)
 H26D(0.7298) H24A(0.7987) H27D(0.735) H27E(0.7085) H27F(0.6842) H25D(0.8)
 H25E(0.842) H25F(0.8363) H21D(0.7219) H21E(0.7693) H21F(0.7294) H20A(0.8092)
 H22C(0.829) H22D(0.7867) H23D(0.8263) H23E(0.8678) H23F(0.8707) H11C(0.4151)
 H11D(0.4559) H9A(0.4417) H10D(0.5265) H10E(0.4862) H10F(0.5296) H12D(0.3634)
 H12E(0.3995) H12F(0.4104) H13A(0.4498) H15C(0.4813) H15D(0.4349) H14D(0.5306)
 H14E(0.4972) H14F(0.5424) H16D(0.386) H16E(0.4318) H16F(0.3969)
;
_olex2_submission_special_instructions 'No special instructions were received'