Picture of a chelate in exchange: the crystal structure of NaHoDOTMA, a 'semi'-hydrated chelate
Katherine M. Payne; Edward J. Valente; Silvio Aime; Mauro Botta; Mark Woods; Chem.Commun. 49 (2013) 2320–; doi:10.1039/c3cc38814j

data_7108965
_publ_section_title
;
 Picture of a chelate in exchange: the crystal structure of NaHoDOTMA, a
 'semi'-hydrated chelate
;
_journal_name_full               Chem.Commun.
_journal_page_first              2320
_journal_paper_doi               10.1039/c3cc38814j
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C40 H72 Cl1 Ho2 N8 Na3 O32'
_chemical_formula_sum            'C40 H72 Cl Ho2 N8 Na3 O32'
_chemical_formula_weight         1611.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           21
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2 2'
_symmetry_space_group_name_H-M   'C 2 2 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5845(3)
_cell_length_b                   18.6061(6)
_cell_length_c                   18.9964(4)
_cell_measurement_reflns_used    12266
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      3
_cell_volume                     6568.7(3)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 16.0309
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34228
_diffrn_reflns_theta_full        30.32
_diffrn_reflns_theta_max         30.32
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.541
_exptl_absorpt_correction_T_max  0.4373
_exptl_absorpt_correction_T_min  0.3018
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3231
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.39
_refine_diff_density_max         2.649
_refine_diff_density_min         -1.715
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         9231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0351P)^2^+22.7032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                7976
_reflns_number_total             9231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc38814j.txt
_cod_data_source_block           up143a
_cod_database_code               7108965