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_4320852
_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            'C58 H56 Cs3 N9 Ni3 O22'
_chemical_formula_weight         1805.98
_chemical_name_common            '[Cs(NO3).Ni(3-MeOsal1,3pn)]3.MeOH'
_chemical_name_systematic
;
 [Caesium nitrate / N.N'-bis(3-methoxysalicylidene)
 propane-1,3-diaminatonickel(II)] (1/1)] /methanol (1/1).
;
_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-97
_cell_angle_alpha                90.0000(1)
_cell_angle_beta                 99.3500(1)
_cell_angle_gamma                90.0000(1)
_cell_formula_units_Z            4
_cell_length_a                   12.5910(2)
_cell_length_b                   23.4880(2)
_cell_length_c                   22.6660(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     6614.13(13)
_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 0.921
_diffrn_measured_fraction_theta_max 0.921
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12922
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    2.555
_exptl_crystal_colour            Deep_Green
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.221
_refine_diff_density_min         -2.035
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         11931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2100
_reflns_number_gt                7180
_reflns_number_total             11931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990496p_7.cif
_cod_data_source_block           '[Cs(NO3).NiL4]3.MeOH'
_cod_database_code               4320852