Polyurethane based organic macromolecular contrast agents (PU-ORCAs) for magnetic resonance imaging
Garmendia, Sofiem; Mantione, Daniele; Alonso-de Castro, Silvia; Jehanno, Coralie; Lezama, Luis; Hedrick, James L.; Mecerreyes, David; Salassa, Luca; Sardon, Haritz; Polym. Chem. 8 (2017) 2693–; doi:10.1039/C7PY00166E

data_1545658
_publ_section_title
;
 Polyurethane based organic macromolecular contrast agents (PU-ORCAs) for
 magnetic resonance imaging
;
_journal_issue                   17
_journal_name_full               'Polym. Chem.'
_journal_page_first              2693
_journal_paper_doi               10.1039/C7PY00166E
_journal_volume                  8
_journal_year                    2017
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C17 H30 N1 O5'
_chemical_formula_sum            'C17 H30 N O5'
_chemical_formula_weight         328.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-03-01T11:25:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-03-16 deposited with the CCDC.
2017-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.5020(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1821(2)
_cell_length_b                   6.16924(7)
_cell_length_c                   17.8483(2)
_cell_measurement_reflns_used    9237
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.346
_cell_measurement_theta_min      3.116
_cell_measurement_wavelength     1.54184
_cell_volume                     1814.00(4)
_computing_cell_refinement
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_collection
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_reduction
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'OLEX2 (Dolomanov et al, 2009)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -72.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9506  -47.0000 -101.0000 57

  2 omega   15.00   78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9506 -125.0000 -120.0000 63

  3 omega  -29.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9506  -37.0000    0.0000 84

  4 omega -150.00  -91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000 -111.0000    0.0000 59

  5 omega   37.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -90.0000 28

  6 omega   34.00  142.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  150.0000 108

  7 omega   45.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 32

  8 omega   38.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  150.0000 31

  9 omega   35.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -120.0000 34

 10 omega   45.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -30.0000 32

 11 omega   35.00   66.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 31

 12 omega   36.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 32

 13 omega   79.00  148.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000 -180.0000 69

 14 omega   49.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000   60.0000 49

 15 omega   14.00   40.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9506   19.0000 -180.0000 26

 16 omega   56.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9506   19.0000 -180.0000 64

 17 omega  -79.00  -38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  178.0000  150.0000 41

 18 omega -156.00 -100.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  178.0000  150.0000 56

 19 omega  -44.00  -18.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   30.0000   30.0000 26

 20 omega   84.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -180.0000 27

 21 omega   33.00   89.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000  120.0000 56

 22 omega   35.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 33

 23 omega   82.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   30.0000 27

 24 omega   64.00  116.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000    0.0000 52

 25 omega  127.00  153.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   30.0000 26

 26 omega   38.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -180.0000 26

 27 omega   94.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -180.0000 64

 28 omega   81.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -150.0000 26

 29 omega   39.00   65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 26

 30 omega   94.00  147.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   90.0000 53

 31 omega   83.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000   60.0000 25

 32 omega   53.00  104.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -30.0000 51
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0047432
_diffrn_orient_matrix_UB_12      0.2068542
_diffrn_orient_matrix_UB_13      -0.0468774
_diffrn_orient_matrix_UB_21      -0.0714841
_diffrn_orient_matrix_UB_22      0.0978331
_diffrn_orient_matrix_UB_23      0.0246534
_diffrn_orient_matrix_UB_31      0.060072
_diffrn_orient_matrix_UB_32      0.1000069
_diffrn_orient_matrix_UB_33      0.0728034
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) X-ray micro-source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14777
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.986
_diffrn_reflns_theta_min         3.151
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.4142
_exptl_crystal_size_mid          0.2117
_exptl_crystal_size_min          0.1633
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.4880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                3176
_reflns_number_total             3429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py00166e2.cif
_cod_data_source_block           a20160058_tempodiol
_cod_depositor_comments          'Adding full bibliography for 1545658.cif.'
_cod_original_cell_volume        1813.99(4)
_cod_database_code               1545658