H4octapa: Synthesis, Solution Equilibria and Complexes with Useful Radiopharmaceutical Metal Ions
Jaraquemada-Peláez, María de Guadalupe; Wang, Xiaozhu; Clough, Thomas J.; Cao, Yang; Choudhary, Neha; Emler, Kirsten; Patrick, Brian O.; Orvig, Chris; Dalton Trans.  (2017) –; doi:10.1039/C7DT02343J

data_7044005
_publ_section_title
;
 H4octapa: Synthesis, Solution Equilibria and Complexes with Useful
 Radiopharmaceutical Metal Ions
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02343J
_journal_year                    2017
_chemical_formula_moiety         'C40 H46.3 La2.5 N8 Na0.5 O21.15, 5(H2 O)'
_chemical_formula_sum            'C40 H56.29 La2.5 N8 Na0.5 O26.15'
_chemical_formula_weight         1426.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-27 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                82.406(5)
_cell_angle_beta                 84.822(5)
_cell_angle_gamma                90.092(4)
_cell_formula_units_Z            2
_cell_length_a                   8.703(3)
_cell_length_b                   16.076(6)
_cell_length_c                   20.536(7)
_cell_measurement_reflns_used    5987
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      2.36
_cell_volume                     2836.1(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8861
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.283
_diffrn_reflns_theta_min         1.278
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 2:
 wR2(int) was 0.0728 before and 0.0624 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 26539 reflections, Rint = 0.0648
 (12126 with I > 3sig(I), Rint = 0.0529)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       blade
_exptl_crystal_F_000             1419
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.956
_refine_diff_density_min         -2.278
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         8861
_refine_ls_number_restraints     1541
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+69.4212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7402
_reflns_number_total             8861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02343j2.cif
_cod_data_source_block           mo_co525_sq
_cod_original_cell_volume        2835.9(17)
_cod_original_formula_sum        'C40 H56.29 La2.50 N8 Na0.50 O26.15'
_cod_database_code               7044005
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.3837(15)
 0.6163(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O1A-H1AA = O1A-H1AB
 0.84 with sigma of 0.01
 O1B-H1BA = O1B-H1BB
 0.84 with sigma of 0.01
 O1C-H1CA = O1C-H1CB
 0.84 with sigma of 0.01
 H1AB-La3A
 -3 with sigma of 0.01
 H1AA-La3A
 -3 with sigma of 0.01
 H1BB-La3
 -3 with sigma of 0.01
 H1BA-La3
 -3 with sigma of 0.01
 H1CB-La3A
 -3 with sigma of 0.01
 H1CA-La3A
 -3 with sigma of 0.01
 H1AA-H1AB
 1.33 with sigma of 0.02
 H1BA-H1BB
 1.33 with sigma of 0.02
 H1CA-H1CB
 1.33 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(Na1) \\sim Ueq, Uanis(Na1A) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(C25) \\sim Ueq, Uanis(O1C) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.014
Uanis(O1C) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.12
Uanis(O17A) = Uanis(O17)
Uanis(O18A) = Uanis(O18)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O17A)=Sof(O18A)=1-FVAR(1)
 Sof(O17)=Sof(O18)=FVAR(1)
 Sof(La3A)=0.5*(1-FVAR(3))
 Sof(La3)=0.5*FVAR(3)
 Sof(O1B)=Sof(H1BA)=Sof(H1BB)=FVAR(3)
 Sof(O1C)=Sof(H1CA)=Sof(H1CB)=FVAR(4)
 Fixed Sof: Na1(0.25) Na1A(0.25) O1A(0.33333) H1AA(0.33333) H1AB(0.33333)
7.a Free rotating group:
 O23(H23A,H23B), O24(H24A,H24B), O25(H25A,H25B), O26(H26A,H26B), O1A(H1AA,
 H1AB), O1B(H1BA,H1BB), O1C(H1CA,H1CB), O10(H10C,H10D), O22(H22A,H22B)
7.b Rotating group:
 O9(H9A,H9B), O20(H20A,H20B), O19(H19A,H19B)
7.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C34(H34A,H34B)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C16(H16), C17(H17), C18(H18), C23(H23), C24(H24),
 C25(H25), C36(H36), C37(H37), C38(H38)
7.e Fitted hexagon refined as free rotating group:
 N1(C2,C3,C4,C5,C6), N4(C15,C16,C17,C18,C19), N5(C22,C23,C24,C25,C26), N8(C35,
 C36,C37,C38,C39)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              9412
_shelx_fab_checksum              98237
_olex2_submission_special_instructions 'No special instructions were received'