Synthesis and structural characterization of complexes of a DO3A-conjugated triphenylphosphonium cation with diagnostically important metal ions.
Yang, Chang-Tong; Li, Yongxin; Liu, Shuang; Inorganic chemistry 46 (2007) 8988–8997; doi:10.1021/ic7010452

data_4339554
_publ_section_title
;
 Synthesis and structural characterization of complexes of a
 DO3A-conjugated triphenylphosphonium cation with diagnostically important
 metal ions.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8988
_journal_page_last               8997
_journal_paper_doi               10.1021/ic7010452
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C40 H46 Ga1 N4 O6 P1,6(H2 O1),N1 O3,C3 H6 O1'
_chemical_formula_sum            'C43 H64 Ga N5 O16 P'
_chemical_formula_weight         1007.71
_chemical_name_systematic        ' ?'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.9585(9)
_cell_length_b                   8.15090(10)
_cell_length_c                   19.6548(6)
_cell_measurement_reflns_used    18858
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     4639.3(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 1997)
;
_computing_publication_material  'SHELX97(Sheldrick, 1997) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution
;
 Direct methods (SIR2004, Burla et al., 2005)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.9842
_diffrn_measured_fraction_theta_max 0.9229
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18858
_diffrn_reflns_theta_full        20.2
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.8116
_exptl_absorpt_correction_T_min  0.7733
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.39
_refine_ls_abs_structure_details
'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.506(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         8697
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.094
_refine_ls_wR_factor_ref         0.100
_reflns_Friedel_coverage         0.8398
_reflns_number_gt                6895
_reflns_number_total             8697
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic7010452-file005.cif
_cod_data_source_block           GADPT
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
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 
;
_cod_original_formula_sum        'C43 H64 Ga1 N5 O16 P1'
_cod_database_code               4339554
_exptl_absorpt_correction_details 'SCALEPACK (Otwinowski & Minor, 1997)'