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#$Date: 2016-03-22 23:58:59 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179087 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/49/4304901.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_4304901
loop_
_publ_author_name
'Yan-Si Jiang'
'Hua-Gang Yao'
'Shou-Hua Ji'
'Min Ji'
'Yong-Lin An'
_publ_section_title
;
New Framework Iodoargentates: M(en)3Ag2I4 (M = Zn, Ni) with Tridymite
Topology
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3922
_journal_page_last               3924
_journal_paper_doi               10.1021/ic7025158
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C6 H24 Ag2 I4 N6 Ni'
_chemical_formula_weight         962.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.9969(2)
_cell_length_b                   8.9969(2)
_cell_length_c                   14.4374(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1012.06(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7767
_diffrn_reflns_theta_full        36.36
_diffrn_reflns_theta_max         36.36
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    8.935
_exptl_crystal_density_diffrn    3.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_refine_diff_density_max         1.063
_refine_diff_density_min         -2.885
_refine_diff_density_rms         0.321
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_coef       0.0195(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         3171
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0360
_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/[σ²(Fo²)+(0.0317P)²+0.5081P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                2552
_reflns_number_total             3171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7025158-file002.cif
_cod_data_source_block           1
_cod_database_code               4304901
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
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
Ag2 Ag 0.6667 0.3333 0.47698(6) 0.0501(2) Uani 1 3 d S . .
I2 I 0.6667 0.3333 0.67648(5) 0.02871(10) Uani 1 3 d S . .
Ni1 Ni 1.0000 1.0000 0.67650(14) 0.02194(13) Uani 1 3 d S . .
I1 I 0.99996(4) 0.60273(4) 0.42649(5) 0.03581(9) Uani 1 1 d . . .
Ag1 Ag 1.3333 0.6667 0.37611(6) 0.0498(2) Uani 1 3 d S . .
N1 N 1.1887(6) 1.2066(6) 0.7568(3) 0.0292(9) Uani 1 1 d . . .
H1A H 1.1420 1.2159 0.8100 0.035 Uiso 1 1 calc R . .
H1D H 1.2749 1.1870 0.7708 0.035 Uiso 1 1 calc R . .
N2 N 1.0173(6) 1.2066(6) 0.5969(3) 0.0291(9) Uani 1 1 d . . .
H2A H 1.0731 1.2161 0.5436 0.035 Uiso 1 1 calc R . .
H2D H 0.9114 1.1868 0.5831 0.035 Uiso 1 1 calc R . .
C1 C 1.2551(6) 1.3665(6) 0.7026(3) 0.0301(9) Uani 1 1 d . . .
H1B H 1.3416 1.3753 0.6593 0.036 Uiso 1 1 calc R . .
H1C H 1.3081 1.4647 0.7438 0.036 Uiso 1 1 calc R . .
C2 C 1.1106(6) 1.3664(6) 0.6507(3) 0.0309(9) Uani 1 1 d . . .
H2B H 1.0330 1.3754 0.6940 0.037 Uiso 1 1 calc R . .
H2C H 1.1557 1.4644 0.6093 0.037 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag2 0.0481(4) 0.0481(4) 0.0541(6) 0.000 0.000 0.02406(19)
I2 0.02840(13) 0.02840(13) 0.02934(17) 0.000 0.000 0.01420(7)
Ni1 0.01927(18) 0.01927(18) 0.0273(3) 0.000 0.000 0.00963(9)
I1 0.03002(14) 0.03948(16) 0.03480(12) 0.00224(16) 0.00431(13) 0.01502(12)
Ag1 0.0479(4) 0.0479(4) 0.0538(6) 0.000 0.000 0.02393(19)
N1 0.028(2) 0.028(2) 0.033(2) -0.0022(14) -0.0053(14) 0.0149(17)
N2 0.0265(19) 0.026(2) 0.035(2) 0.0004(14) -0.0054(14) 0.0135(16)
C1 0.0242(19) 0.0206(18) 0.039(2) -0.0008(14) -0.0003(15) 0.0061(16)
C2 0.030(2) 0.0221(19) 0.044(2) 0.0029(15) 0.0036(17) 0.0156(17)
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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'
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
I1 Ag2 I1 113.70(2) 3_665 . ?
I1 Ag2 I1 113.70(2) 3_665 2_655 ?
I1 Ag2 I1 113.70(2) . 2_655 ?
I1 Ag2 I2 104.81(3) 3_665 . ?
I1 Ag2 I2 104.81(3) . . ?
I1 Ag2 I2 104.81(3) 2_655 . ?
Ag2 I2 Ag1 180.0 . 4_765 ?
N2 Ni1 N2 93.50(19) 2_765 . ?
N2 Ni1 N2 93.50(19) 2_765 3_675 ?
N2 Ni1 N2 93.50(19) . 3_675 ?
N2 Ni1 N1 172.61(17) 2_765 . ?
N2 Ni1 N1 81.54(14) . . ?
N2 Ni1 N1 92.27(16) 3_675 . ?
N2 Ni1 N1 81.54(14) 2_765 2_765 ?
N2 Ni1 N1 92.27(16) . 2_765 ?
N2 Ni1 N1 172.61(17) 3_675 2_765 ?
N1 Ni1 N1 93.14(18) . 2_765 ?
N2 Ni1 N1 92.27(16) 2_765 3_675 ?
N2 Ni1 N1 172.61(17) . 3_675 ?
N2 Ni1 N1 81.54(14) 3_675 3_675 ?
N1 Ni1 N1 93.14(18) . 3_675 ?
N1 Ni1 N1 93.14(18) 2_765 3_675 ?
Ag2 I1 Ag1 142.166(12) . . ?
I1 Ag1 I1 113.73(2) 3_775 . ?
I1 Ag1 I1 113.73(2) 3_775 2_755 ?
I1 Ag1 I1 113.73(2) . 2_755 ?
I1 Ag1 I2 104.78(3) 3_775 4_764 ?
I1 Ag1 I2 104.78(3) . 4_764 ?
I1 Ag1 I2 104.78(3) 2_755 4_764 ?
C1 N1 Ni1 108.7(3) . . ?
C2 N2 Ni1 109.0(3) . . ?
N1 C1 C2 109.6(4) . . ?
N2 C2 C1 109.5(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
Ag2 I1 2.8512(4) 3_665 ?
Ag2 I1 2.8512(4) . ?
Ag2 I1 2.8512(4) 2_655 ?
Ag2 I2 2.8803(12) . ?
I2 Ag1 2.8821(12) 4_765 ?
Ni1 N2 2.123(5) 2_765 ?
Ni1 N2 2.123(5) . ?
Ni1 N2 2.123(5) 3_675 ?
Ni1 N1 2.127(5) . ?
Ni1 N1 2.127(5) 2_765 ?
Ni1 N1 2.127(5) 3_675 ?
I1 Ag1 2.8514(4) . ?
Ag1 I1 2.8514(4) 3_775 ?
Ag1 I1 2.8514(4) 2_755 ?
Ag1 I2 2.8821(12) 4_764 ?
N1 C1 1.477(6) . ?
N2 C2 1.472(6) . ?
C1 C2 1.500(6) . ?
