Hafnium-Based Contrast Agents for X-ray Computed Tomography.
Berger, Markus; Bauser, Marcus; Frenzel, Thomas; Hilger, Christoph Stephan; Jost, Gregor; Lauria, Silvia; Morgenstern, Bernd; Neis, Christian; Pietsch, Hubertus; Sülzle, Detlev; Hegetschweiler, Kaspar; Inorganic chemistry 56 (2017) 5757–5761; doi:10.1021/acs.inorgchem.7b00359

data_4345738
_publ_section_title
;
 Hafnium-Based Contrast Agents for X-ray Computed Tomography.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5757
_journal_page_last               5761
_journal_paper_doi               10.1021/acs.inorgchem.7b00359
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C28 H68 Hf3 N6 O33'
_chemical_formula_weight         1552.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.598(3)
_cell_length_b                   18.186(4)
_cell_length_c                   20.913(4)
_cell_measurement_reflns_used    8247
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      44.32
_cell_measurement_theta_min      2.25
_cell_volume                     4791.3(18)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'DIAMOND, Vers. 3.2i (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 Apex, Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            145730
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.505
_diffrn_reflns_theta_min         1.484
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.592
_exptl_absorpt_correction_T_max  0.2896
_exptl_absorpt_correction_T_min  0.1554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2010)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.673
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 7157 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0111(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         15962
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0154
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0051P)^2^+5.8852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.0368
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15870
_reflns_number_total             15962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00359_si_003.cif
_cod_data_source_block           sh3382
_cod_depositor_comments
'Adding full bibliography for 4345737--4345739.cif.'
_cod_original_cell_volume        4791.2(17)
_cod_database_code               4345738
_shelx_estimated_absorpt_t_min   0.155
_shelx_estimated_absorpt_t_max   0.290
_shelxl_version_number           2014/6
_shelx_res_checksum              22489
_shelx_hkl_checksum              43370