Metal Complexes of Tetrapodal Ligands: Synthesis, Spectroscopic and Thermal Studies, and X-ray Crystal Structure Studies of Na(I), Ca(II), Sr(II), and Ba(II) Complexes of Tetrapodal Ligands N,N,N',N'-Tetrakis(2-hydroxypropyl)ethylenediamine and N,N,N',N'-Tetrakis(2-hydroxyethyl)ethylenediamine
Geeta Hundal; Maninder Singh Hundal; Sangeeta Obrai; N. S. Poonia; Subodh Kumar; Inorganic Chemistry 41 (2002) 2077–2086; doi:10.1021/ic0100727

data_4317834
_publ_section_title
;
 Metal Complexes of Tetrapodal Ligands: Synthesis, Spectroscopic and
 Thermal Studies, and X-ray Crystal Structure Studies of Na(I), Ca(II),
 Sr(II), and Ba(II) Complexes of Tetrapodal Ligands
 N,N,N',N'-Tetrakis(2-hydroxypropyl)ethylenediamine and
 N,N,N',N'-Tetrakis(2-hydroxyethyl)ethylenediamine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2077
_journal_page_last               2086
_journal_paper_doi               10.1021/ic0100727
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C28 H44 Ba N6 O19'
_chemical_formula_weight         906.03
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 100.45(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.376(2)
_cell_length_b                   18.371(4)
_cell_length_c                   22.549(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3819.6(15)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5120
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.294
_exptl_absorpt_correction_T_min  0.265
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_F_000             1848
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.119
_refine_ls_goodness_of_fit_obs   1.016
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         4438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_restrained_S_obs      1.016
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_obs          0.0374
_refine_ls_shift/esd_max         5.126
_refine_ls_shift/esd_mean        0.473
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+7.1176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1395
_refine_ls_wR_factor_obs         0.1018
_reflns_number_observed          3881
_reflns_number_total             4621
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0100727_08.cif
_cod_data_source_block           badnbhpe
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (36 times).

'_geom_bond_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (9
times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+7.1176P] 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^)+(0.0658P)^2^+7.1176P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3819.6(13)
_cod_database_code               4317834