#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/08/4320848.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320848
loop_
_publ_author_name
'D. Cunningham'
'P. McArdle'
'M. Mitchell'
'N. Ní Chonchubhair'
'M. O'Gara'
'Federico Franceschi'
'Carlo Floriani'
_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/[σ²(Fo²)+(0.1695P)²+0.1172P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.01767(6) 0.17676(5) 0.23858(4) 0.0743(2) Uani 1 1 d . . .
Cs2 Cs 0.0000 0.5000 0.5000 0.04546(18) Uani 1 2 d S . .
Ni1 Ni 0.36161(6) 0.39660(6) 0.38250(5) 0.03351(19) Uani 1 1 d . . .
I2 I 0.0000 0.0000 0.0000 0.04822(19) Uani 1 2 d S . .
O1 O 0.2745(4) 0.5463(3) 0.3757(3) 0.0394(7) Uani 1 1 d . . .
O2 O 0.2896(4) 0.4079(4) 0.5355(3) 0.0428(7) Uani 1 1 d . . .
O3 O 0.1764(4) 0.7778(4) 0.4224(3) 0.0484(9) Uani 1 1 d . . .
O4 O 0.1432(5) 0.4441(5) 0.7318(4) 0.0578(10) Uani 1 1 d . . .
N1 N 0.3941(4) 0.3646(4) 0.2161(3) 0.0371(8) Uani 1 1 d . . .
N2 N 0.4792(4) 0.2738(4) 0.4094(4) 0.0383(8) Uani 1 1 d . . .
C1 C 0.2828(5) 0.6199(5) 0.2904(4) 0.0352(9) Uani 1 1 d . . .
C2 C 0.2300(5) 0.7459(5) 0.3118(4) 0.0392(10) Uani 1 1 d . . .
C3 C 0.2355(7) 0.8263(7) 0.2253(6) 0.0527(13) Uani 1 1 d . . .
H1 H 0.2036 0.9098 0.2419 0.068 Uiso 1 1 calc R . .
C4 C 0.2886(7) 0.7839(7) 0.1122(6) 0.0580(16) Uani 1 1 d . . .
H2 H 0.2910 0.8386 0.0539 0.075 Uiso 1 1 calc R . .
C5 C 0.3370(6) 0.6617(6) 0.0878(5) 0.0484(12) Uani 1 1 d . . .
H3 H 0.3710 0.6331 0.0123 0.063 Uiso 1 1 calc R . .
C6 C 0.3356(5) 0.5789(5) 0.1764(4) 0.0394(9) Uani 1 1 d . . .
C7 C 0.3765(5) 0.4471(5) 0.1441(4) 0.0416(10) Uani 1 1 d . . .
H4 H 0.3922 0.4176 0.0630 0.054 Uiso 1 1 calc R . .
C8 C 0.4138(7) 0.2259(6) 0.1602(5) 0.0489(12) Uani 1 1 d . . .
H5 H 0.4091 0.2165 0.0729 0.064 Uiso 1 1 calc R . .
H6 H 0.3380 0.1579 0.1811 0.064 Uiso 1 1 calc R . .
C9 C 0.5544(7) 0.1961(6) 0.2006(5) 0.0545(13) Uani 1 1 d . . .
H7 H 0.5473 0.0967 0.1918 0.071 Uiso 1 1 calc R . .
H8 H 0.6263 0.2287 0.1484 0.071 Uiso 1 1 calc R . .
C10 C 0.5987(6) 0.2655(6) 0.3314(5) 0.0473(12) Uani 1 1 d . . .
H9 H 0.6612 0.2139 0.3636 0.062 Uiso 1 1 calc R . .
H10 H 0.6510 0.3584 0.3334 0.062 Uiso 1 1 calc R . .
C11 C 0.4740(5) 0.2113(5) 0.4986(4) 0.0403(9) Uani 1 1 d . . .
H11 H 0.5373 0.1521 0.5003 0.052 Uiso 1 1 calc R . .
C12 C 0.3810(5) 0.2226(5) 0.5965(4) 0.0376(9) Uani 1 1 d . . .
C13 C 0.3843(6) 0.1365(6) 0.6811(5) 0.0497(12) Uani 1 1 d . . .
H12 H 0.4414 0.0704 0.6698 0.065 Uiso 1 1 calc R . .
C14 C 0.3042(7) 0.1492(7) 0.7795(6) 0.0581(15) Uani 1 1 d . . .
H13 H 0.3037 0.0893 0.8333 0.075 Uiso 1 1 calc R . .
C15 C 0.2235(7) 0.2520(7) 0.7991(5) 0.0528(13) Uani 1 1 d . . .
H14 H 0.1712 0.2619 0.8677 0.069 Uiso 1 1 calc R . .
C16 C 0.2195(6) 0.3397(6) 0.7188(5) 0.0425(10) Uani 1 1 d . . .
C17 C 0.2967(5) 0.3243(5) 0.6111(4) 0.0379(9) Uani 1 1 d . . .
C18 C 0.1138(9) 0.8989(8) 0.4449(6) 0.0660(17) Uani 1 1 d . . .
H15 H 0.0804 0.9116 0.5252 0.086 Uiso 1 1 calc R . .
H16 H 0.0364 0.8876 0.3871 0.086 Uiso 1 1 calc R . .
H17 H 0.1827 0.9787 0.4373 0.086 Uiso 1 1 calc R . .
C19 C 0.0740(7) 0.4698(8) 0.8422(6) 0.0613(16) Uani 1 1 d . . .
H18 H 0.0239 0.5441 0.8416 0.080 Uiso 1 1 calc R . .
H19 H 0.1425 0.4951 0.9091 0.080 Uiso 1 1 calc R . .
H20 H 0.0090 0.3875 0.8501 0.080 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 I1 Cs2 161.09(2) . . ?
O1 Cs2 O1 180.0 . 2_566 ?
O1 Cs2 O4 86.70(10) . 2_566 ?
O1 Cs2 O4 93.30(10) 2_566 2_566 ?
O1 Cs2 O4 93.30(10) . . ?
O1 Cs2 O4 86.70(10) 2_566 . ?
O4 Cs2 O4 180.000(1) 2_566 . ?
O1 Cs2 O2 47.51(8) . . ?
O1 Cs2 O2 132.49(8) 2_566 . ?
O4 Cs2 O2 130.07(9) 2_566 . ?
O4 Cs2 O2 49.93(9) . . ?
O1 Cs2 O2 132.49(8) . 2_566 ?
O1 Cs2 O2 47.51(8) 2_566 2_566 ?
O4 Cs2 O2 49.93(9) 2_566 2_566 ?
O4 Cs2 O2 130.07(9) . 2_566 ?
O2 Cs2 O2 180.0 . 2_566 ?
O1 Cs2 O3 130.82(9) . 2_566 ?
O1 Cs2 O3 49.18(9) 2_566 2_566 ?
O4 Cs2 O3 110.29(12) 2_566 2_566 ?
O4 Cs2 O3 69.71(12) . 2_566 ?
O2 Cs2 O3 92.24(9) . 2_566 ?
O2 Cs2 O3 87.76(9) 2_566 2_566 ?
O1 Cs2 O3 49.18(9) . . ?
O1 Cs2 O3 130.82(9) 2_566 . ?
O4 Cs2 O3 69.71(12) 2_566 . ?
O4 Cs2 O3 110.29(12) . . ?
O2 Cs2 O3 87.76(9) . . ?
O2 Cs2 O3 92.24(9) 2_566 . ?
O3 Cs2 O3 180.0 2_566 . ?
O1 Cs2 C1 162.34(9) . 2_566 ?
O1 Cs2 C1 17.66(9) 2_566 2_566 ?
O4 Cs2 C1 109.48(11) 2_566 2_566 ?
O4 Cs2 C1 70.52(11) . 2_566 ?
O2 Cs2 C1 114.84(9) . 2_566 ?
O2 Cs2 C1 65.16(9) 2_566 2_566 ?
O3 Cs2 C1 37.69(9) 2_566 2_566 ?
O3 Cs2 C1 142.31(9) . 2_566 ?
O1 Cs2 C1 17.66(9) . . ?
O1 Cs2 C1 162.34(9) 2_566 . ?
O4 Cs2 C1 70.52(11) 2_566 . ?
O4 Cs2 C1 109.48(11) . . ?
O2 Cs2 C1 65.16(9) . . ?
O2 Cs2 C1 114.84(9) 2_566 . ?
O3 Cs2 C1 142.31(9) 2_566 . ?
O3 Cs2 C1 37.69(9) . . ?
C1 Cs2 C1 180.0 2_566 . ?
O1 Cs2 I1 69.66(7) . . ?
O1 Cs2 I1 110.34(7) 2_566 . ?
O4 Cs2 I1 73.86(9) 2_566 . ?
O4 Cs2 I1 106.14(9) . . ?
O2 Cs2 I1 72.12(7) . . ?
O2 Cs2 I1 107.88(7) 2_566 . ?
O3 Cs2 I1 71.63(7) 2_566 . ?
O3 Cs2 I1 108.37(7) . . ?
C1 Cs2 I1 107.23(7) 2_566 . ?
C1 Cs2 I1 72.77(7) . . ?
O1 Cs2 I1 110.34(7) . 2_566 ?
O1 Cs2 I1 69.66(7) 2_566 2_566 ?
O4 Cs2 I1 106.14(9) 2_566 2_566 ?
O4 Cs2 I1 73.86(9) . 2_566 ?
O2 Cs2 I1 107.88(7) . 2_566 ?
O2 Cs2 I1 72.12(7) 2_566 2_566 ?
O3 Cs2 I1 108.37(7) 2_566 2_566 ?
O3 Cs2 I1 71.63(7) . 2_566 ?
C1 Cs2 I1 72.77(7) 2_566 2_566 ?
C1 Cs2 I1 107.23(7) . 2_566 ?
I1 Cs2 I1 180.0 . 2_566 ?
O1 Ni1 O2 83.97(14) . . ?
O1 Ni1 N2 167.88(18) . . ?
O2 Ni1 N2 93.62(16) . . ?
O1 Ni1 N1 93.78(15) . . ?
O2 Ni1 N1 167.41(18) . . ?
N2 Ni1 N1 91.07(17) . . ?
O1 Ni1 Cs2 46.10(10) . . ?
O2 Ni1 Cs2 50.00(11) . . ?
N2 Ni1 Cs2 138.17(12) . . ?
N1 Ni1 Cs2 120.69(12) . . ?
I1 I2 I1 180.00(2) 2 . ?
C1 O1 Ni1 127.1(3) . . ?
C1 O1 Cs2 117.9(3) . . ?
Ni1 O1 Cs2 107.61(13) . . ?
C17 O2 Ni1 127.4(3) . . ?
C17 O2 Cs2 117.7(3) . . ?
Ni1 O2 Cs2 103.07(14) . . ?
C2 O3 C18 116.7(5) . . ?
C2 O3 Cs2 110.8(3) . . ?
C18 O3 Cs2 116.6(4) . . ?
C16 O4 C19 116.4(5) . . ?
C16 O4 Cs2 118.4(3) . . ?
C19 O4 Cs2 117.3(4) . . ?
C7 N1 C8 116.9(4) . . ?
C7 N1 Ni1 124.8(3) . . ?
C8 N1 Ni1 117.1(3) . . ?
C11 N2 C10 117.5(4) . . ?
C11 N2 Ni1 125.2(3) . . ?
C10 N2 Ni1 116.7(3) . . ?
O1 C1 C6 123.8(4) . . ?
O1 C1 C2 118.5(4) . . ?
C6 C1 C2 117.6(4) . . ?
O1 C1 Cs2 44.4(2) . . ?
C6 C1 Cs2 141.8(3) . . ?
C2 C1 Cs2 84.8(3) . . ?
O3 C2 C3 124.4(5) . . ?
O3 C2 C1 114.8(4) . . ?
C3 C2 C1 120.8(5) . . ?
C2 C3 C4 120.8(5) . . ?
C5 C4 C3 119.8(5) . . ?
C4 C5 C6 120.5(5) . . ?
C1 C6 C5 120.5(4) . . ?
C1 C6 C7 120.6(4) . . ?
C5 C6 C7 118.7(4) . . ?
N1 C7 C6 126.8(4) . . ?
N1 C8 C9 112.2(5) . . ?
C10 C9 C8 112.4(4) . . ?
N2 C10 C9 113.2(5) . . ?
N2 C11 C12 127.1(5) . . ?
C17 C12 C13 121.3(5) . . ?
C17 C12 C11 120.2(4) . . ?
C13 C12 C11 118.4(5) . . ?
C14 C13 C12 120.5(5) . . ?
C13 C14 C15 119.8(5) . . ?
C16 C15 C14 121.2(5) . . ?
O4 C16 C15 124.8(5) . . ?
O4 C16 C17 114.8(5) . . ?
C15 C16 C17 120.4(5) . . ?
O2 C17 C12 124.0(4) . . ?
O2 C17 C16 119.1(4) . . ?
C12 C17 C16 116.8(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 I2 2.9047(5) . ?
I1 Cs2 3.9666(6) . ?
Cs2 O1 3.027(3) . ?
Cs2 O1 3.027(3) 2_566 ?
Cs2 O4 3.127(4) 2_566 ?
Cs2 O4 3.127(4) . ?
Cs2 O2 3.149(4) . ?
Cs2 O2 3.149(4) 2_566 ?
Cs2 O3 3.262(4) 2_566 ?
Cs2 O3 3.262(4) . ?
Cs2 C1 3.822(5) 2_566 ?
Cs2 C1 3.822(5) . ?
Cs2 I1 3.9666(6) 2_566 ?
Ni1 O1 1.861(3) . ?
Ni1 O2 1.862(3) . ?
Ni1 N2 1.881(4) . ?
Ni1 N1 1.883(4) . ?
I2 I1 2.9047(5) 2 ?
O1 C1 1.313(5) . ?
O2 C17 1.312(6) . ?
O3 C2 1.362(6) . ?
O3 C18 1.434(7) . ?
O4 C16 1.373(7) . ?
O4 C19 1.425(6) . ?
N1 C7 1.293(6) . ?
N1 C8 1.457(7) . ?
N2 C11 1.278(6) . ?
N2 C10 1.470(6) . ?
C1 C6 1.406(6) . ?
C1 C2 1.426(7) . ?
C2 C3 1.373(7) . ?
C3 C4 1.401(8) . ?
C4 C5 1.369(8) . ?
C5 C6 1.413(7) . ?
C6 C7 1.428(7) . ?
C8 C9 1.526(9) . ?
C9 C10 1.522(9) . ?
C11 C12 1.436(7) . ?
C12 C17 1.404(7) . ?
C12 C13 1.405(7) . ?
C13 C14 1.363(9) . ?
C14 C15 1.389(10) . ?
C15 C16 1.381(8) . ?
C16 C17 1.434(7) . ?
