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_4320851
_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            'C38 H40 Cs I N4 Ni2 O9'
_chemical_formula_weight         1073.97
_chemical_name_common            'CsI.[Ni (3-MeOsal1,2pn)]2.H2O'
_chemical_name_systematic
;
 [Caesium iodide / N.N'-bis(3-methoxysalicylidene)
 propane-1,2-diaminato nickel(II) (1/2)] / water (1/1)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   15.752(3)
_cell_length_b                   23.276(8)
_cell_length_c                   25.206(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     9242(4)
_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 0.894
_diffrn_measured_fraction_theta_max 0.894
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7864
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    2.310
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Multi-faced Block'
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.180
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.0719
_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^)+(0.1518P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2308
_reflns_number_gt                3478
_reflns_number_total             7248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990496p_6.cif
_cod_data_source_block           CsI.Ni(L2)2.H2O
_cod_database_code               4320851