Properties, Solution State Behavior, and Crystal Structures of Chelates of DOTMA
Silvio Aime; Mauro Botta; Zoltán Garda; Benjamin E. Kucera; Gyula Tircso; Victor G. Young; Mark Woods; Inorganic Chemistry 50 (2011) 7955–7965; doi:10.1021/ic2012827

data_4326197
_publ_section_title
;
 Properties, Solution State Behavior, and Crystal Structures of Chelates
 of DOTMA
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7955
_journal_page_last               7965
_journal_paper_doi               10.1021/ic2012827
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration adrm
_chemical_formula_moiety
'C20 H39 Gd N4 O9, 2(Na), 4(H2 O), 2(Cl), 17(O)'
_chemical_formula_sum            'C20 H43 Cl Gd N4 Na2 O15'
_chemical_formula_weight         818.26
_chemical_name_common            08123zz
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           3
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2y'
_symmetry_space_group_name_H-M   'P 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.266(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6639(12)
_cell_length_b                   9.6379(12)
_cell_length_c                   18.926(2)
_cell_measurement_reflns_used    3658
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.38
_cell_volume                     1744.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18679
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    2.067
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008/1)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       Block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7882
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+2.4901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                7068
_reflns_number_total             7882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012827_si_001.cif
_cod_data_source_block           08123zz
_cod_depositor_comments
;

2021-10-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H86 Cl2 Gd2 N8 Na4 O30'
_cod_original_formula_weight         1636.53
_cod_original_formula_moiety
'C40 H78 Gd2 N8 Na4 O23, 4(H2 O), 2(Cl), 3(O)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1744.5(4)
_cod_original_sg_symbol_H-M      'P 2'
_cod_database_code               4326197