Structural, kinetic, and thermodynamic characterization of the interconverting isomers of MS-325, a gadolinium(III)-based magnetic resonance angiography contrast agent.
Tyeklar, Zoltan; Dunham, Stephen U.; Midelfort, Katarina; Scott, Daniel M.; Sajiki, Hirano; Ong, Karen; Lauffer, Randall B.; Caravan, Peter; McMurry, Thomas J.; Inorganic chemistry 46 (2007) 6621–6631; doi:10.1021/ic7006843

data_4339282
_publ_section_title
;
 Structural, kinetic, and thermodynamic characterization of the
 interconverting isomers of MS-325, a gadolinium(III)-based magnetic
 resonance angiography contrast agent.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6621
_journal_page_last               6631
_journal_paper_doi               10.1021/ic7006843
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C39 H95.78 Co Gd N9 O30.89 P'
_chemical_formula_weight         1432.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   41.7541(3)
_cell_length_b                   41.7541(3)
_cell_length_c                   9.42520(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.5
_cell_volume                     14230.5(2)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT / SADABS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method       '\w scans 0.3 per frame, 30 sec per frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.1038
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            56045
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         0.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.417
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type
'empirical based on redundant measurements SADA'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    none
_exptl_crystal_description       needlelike
_exptl_crystal_F_000             6713
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2220
_refine_ls_number_reflns         32765
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      1.150
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_obs          0.0568
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1088
_refine_ls_wR_factor_obs         0.0947
_reflns_number_observed          28805
_reflns_number_total             32769
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic7006843-file002.cif
_cod_data_source_block           ztxx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P3(2)
_cod_database_code               4339282