Adduct Formation between Alkali Metal Ions and Divalent Metal Salicylaldimine Complexes Having Methoxy Substituents. A Structural Investigation
D. Cunningham; P. McArdle; M. Mitchell; N. Ní Chonchubhair; M. O'Gara; Federico Franceschi; Carlo Floriani; Inorganic Chemistry 39 (2000) 1639–1649; doi:10.1021/ic990496p

data_4320848
_publ_section_title
;
 Adduct Formation between Alkali Metal Ions and Divalent Metal
 Salicylaldimine Complexes Having Methoxy Substituents. A Structural
 Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1639
_journal_page_last               1649
_journal_paper_doi               10.1021/ic990496p
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C19 H20 Cs0.5 I1.5 N2 Ni O4'
_chemical_formula_weight         655.89
_chemical_name_common            CsI3.Ni(3-MeOsal1,3pn)
_chemical_name_systematic
;
 Caesium triiodide / N.N'-bis(3-methoxysalicylidene)
 propane-1,3-diaminato nickel(II) (1/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.03
_cell_angle_beta                 90.97
_cell_angle_gamma                100.55
_cell_formula_units_Z            2
_cell_length_a                   9.6809(11)
_cell_length_b                   10.0015(13)
_cell_length_c                   11.2686(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1051.3(2)
_computing_cell_refinement       'CELDIM in CAD4-PC-Software'
_computing_data_collection       'CAD4-PC-Software (Enraf-Nonius, 1992)'
_computing_data_reduction        'XCAD (McArdle & Higgins, 1995)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.660
_diffrn_measured_fraction_theta_max 0.660
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0106
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5141
_diffrn_reflns_theta_full        31.96
_diffrn_reflns_theta_max         31.96
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    4.006
_exptl_crystal_colour            Ruby
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.926
_refine_diff_density_min         -2.335
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1695P)^2^+0.1172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2045
_reflns_number_gt                4056
_reflns_number_total             4809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990496p_3.cif
_cod_data_source_block           CsI3.(NiL4)2.H2O
_cod_original_formula_sum        'C19 H20 Cs0.50 I1.50 N2 Ni O4'
_cod_database_code               4320848