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#$Date: 2016-03-23 15:42:34 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179343 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/40/4324031.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_4324031
loop_
_publ_author_name
'Hidetaka Yuge'
'Yohsuke Noda'
'Toschitake Iwamoto'
_publ_section_title
;
 Variations in Catenation Behavior in Aromatic Guest Clathrates Containing
 Rigid Host Entitiesp-Xylylenediamine (p-xda) and Tetracyanonickelate(II)
 Linking Octahedral Cadmium(II) in [Cd(p-xda)nNi(CN)4] Host (n= 1, 1.5, or
 2) and the Related Complex [Cd(C6H5NH2)2(p-xda)Ni(CN)4]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1842
_journal_page_last               1848
_journal_paper_doi               10.1021/ic950382n
_journal_volume                  35
_journal_year                    1996
_chemical_formula_moiety         'C20 H24 Cd N8 Ni, (C7 H9 N)'
_chemical_formula_structural     'Cd (C4 N4 Ni) (C8 H12 N2)2 (C7 H9 N)'
_chemical_formula_sum            'C27 H33 Cd N9 Ni'
_chemical_formula_weight         654.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                81.03(1)
_cell_angle_beta                 94.08(2)
_cell_angle_gamma                106.08(2)
_cell_formula_units_Z            1
_cell_length_a                   8.149(2)
_cell_length_b                   9.577(1)
_cell_length_c                   9.865(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      17.50
_cell_measurement_theta_min      17.06
_cell_volume                     730.4(3)
_diffrn_measurement_device       'RIGAKU AFC5R diffractometer'
_diffrn_measurement_method       '2\q-\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70926
_diffrn_reflns_av_R_equivalents  0.012
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4600
_diffrn_reflns_theta_max         30.00
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.404
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.49
_exptl_crystal_density_meas      1.47(1)
_exptl_crystal_density_method    'flotation in mesitylene-bromoform'
_exptl_crystal_description       flaky
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.16
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.178
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3285
_refine_ls_R_factor_obs          0.0490
_refine_ls_shift/esd_max         0.016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0567
_reflns_number_observed          3285
_reflns_number_total             3943
_reflns_observed_criterion       >4sigma(F)
_cod_data_source_file            ic950382n_2.cif
_cod_data_source_block           compound_(2)
_cod_original_cell_volume        730.4(2)
_cod_database_code               4324031
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cd .0310(3) .0250(3) .0420(3) -.0012(2) .0024(2) -.0084(2)
Ni .0335(5) .0235(4) .0479(6) -.0035(4) .0049(4) -.0082(4)
N(1) .048(3) .036(3) .063(3) -.008(2) .004(3) -.008(2)
N(2) .066(4) .059(4) .075(4) .026(3) -.001(3) -.018(3)
N(3) .041(3) .047(3) .044(3) .009(2) .002(2) -.012(2)
N(4) .062(3) .047(3) .047(3) .025(3) -.005(2) -.013(2)
C(1) .040(3) .033(3) .048(3) .001(2) .004(2) -.009(2)
C(2) .045(3) .038(3) .050(3) .003(2) .004(3) -.015(3)
C(3) .066(4) .065(4) .054(4) -.013(3) .023(3) -.023(3)
C(4) .042(3) .046(3) .045(3) .007(2) .005(2) -.007(2)
C(5) .082(5) .043(3) .052(4) .001(3) .014(3) -.008(3)
C(6) .080(5) .046(3) .049(4) .014(3) .011(3) -.006(3)
C(7) .037(3) .054(3) .039(3) .020(2) -.004(2) -.004(2)
C(8) .045(3) .048(3) .052(3) .009(3) .006(3) -.001(3)
C(9) .043(3) .046(3) .054(4) .007(3) .005(3) -.006(3)
C(10) .048(3) .078(5) .046(3) .026(3) .000(3) -.016(3)
N(11) .057(6) .055(6) .050(6) .005(5) .019(5) -.006(5)
C(11) .090(11) .032(6) .097(12) .010(7) .051(0) -.003(7)
C(12) .056(7) .038(6) .052(7) .013(5) .013(6) -.005(5)
C(13) .081(6) .037(3) .100(6) .010(4) .007(5) -.014(4)
C(14) .074(10) .051(8) .055(8) .010(7) .010(7) -.007(6)
C(15) .100(7) .058(5) .108(8) .015(5) .024(6) -.015(5)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_calc_attached_atom
Cd 1.0 1.0 .0 .0340(2) Uani 1.0 d .
Ni .5 .5 .0 .0367(3) Uani 1.0 d .
N(1) .7693(7) .7838(5) .0147(6) .053(2) Uani 1.0 d .
N(2) .7518(8) .3296(7) .1129(7) .064(3) Uani 1.0 d .
N(3) .9446(6) 1.0612(5) .2158(5) .044(2) Uani 1.0 d .
N(4) .8297(7) 1.1530(6) .8999(5) .050(2) Uani 1.0 d .
C(1) .6690(7) .6759(6) .0097(6) .042(2) Uani 1.0 d .
C(2) .6563(8) .3937(6) .0712(6) .045(2) Uani 1.0 d .
C(3) .7943(10) .9677(8) .2878(7) .065(3) Uani 1.0 d .
C(4) .7676(8) 1.0023(7) .4284(6) .045(2) Uani 1.0 d .
C(5) .8302(10) 1.1423(7) .4652(7) .061(3) Uani 1.0 d .
C(6) .7961(10) 1.1704(7) .5934(7) .058(3) Uani 1.0 d .
C(7) .7013(7) 1.0603(7) .6864(6) .042(2) Uani 1.0 d .
C(8) .6391(8) .9196(7) .6504(7) .049(2) Uani 1.0 d .
C(9) .6735(8) .8925(7) .5219(7) .048(2) Uani 1.0 d .
C(10) .6651(8) 1.0930(8) .8251(7) .055(3) Uani 1.0 d .
N(11) .1093(14) .4905(12) .2333(11) .056(4) Uani 0.5 d .
C(11) .2415(22) .4820(14) .3560(19) .073(6) Uani 0.5 d .
C(12) .4204(17) .5088(13) .3404(14) .048(4) Uani 0.5 d .
C(13) .5284(12) .5121(8) .4320(9) .073(3) Uani 1.0 d .
C(14) .1901(21) .4563(16) .4933(16) .061(6) Uani 0.5 d .
C(15) .7125(14) .5400(10) .4090(11) .088(4) Uani 1.0 d .
H(1) .93160 1.16337 .19872 .076 Uiso 1.0 calc N(3)
H(2) 1.04647 1.05860 .27805 .076 Uiso 1.0 calc N(3)
H(3) .68129 .97638 .22262 .076 Uiso 1.0 calc C(3)
H(4) .80417 .85410 .30076 .076 Uiso 1.0 calc C(3)
H(5) .90578 1.22983 .39404 .076 Uiso 1.0 calc C(5)
H(6) .84469 1.27986 .62010 .076 Uiso 1.0 calc C(6)
H(7) .56439 .83182 .72178 .076 Uiso 1.0 calc C(8)
H(8) .62534 .78298 .49514 .076 Uiso 1.0 calc C(9)
H(9) .59184 .99125 .88571 .076 Uiso 1.0 calc C(10)
H(10) .59042 1.17416 .81023 .076 Uiso 1.0 calc C(10)
H(11) .90275 1.23035 .83278 .076 Uiso 1.0 calc N(4)
H(12) .80078 1.19951 .97572 .076 Uiso 1.0 calc N(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_2
_geom_angle_site_symmetry_3
C(1) Ni C(2) 90.1(2) . . .
N(1) Cd N(3) 94.0(2) . . .
N(1) Cd N(4) 93.8(2) . . .
N(3) Cd N(4) 86.3(2) . . .
Ni C(1) N(1) 178.8(6) . . .
Ni C(2) N(2) 179.2(6) . . .
Cd N(1) C(1) 171.6(5) . . .
Cd N(3) C(3) 117.3(4) . . .
Cd N(4) C(10) 121.2(4) . 1_554 1_554
N(3) C(3) C(4) 116.5(5) . . .
C(3) C(4) C(5) 122.4(6) . . .
C(3) C(4) C(9) 119.0(6) . . .
C(5) C(4) C(9) 118.5(6) . . .
C(4) C(5) C(6) 120.4(6) . . .
C(5) C(6) C(7) 120.9(6) . . .
C(6) C(7) C(8) 118.9(6) . . .
C(6) C(7) C(10) 120.1(6) . . .
C(8) C(7) C(10) 121.0(6) . . .
C(7) C(8) C(9) 119.9(6) . . .
C(4) C(9) C(8) 121.4(6) . . .
C(7) C(10) N(4) 109.8(5) . . .
N(11) C(11) C(12) 124.2(13) . . .
N(11) C(11) C(14) 121.0(14) . . .
C(12) C(11) C(14) 114.7(17) . . .
C(11) C(12) C(13) 126.5(13) . . .
C(12) C(13) C(15) 123.9(10) . . .
C(12) C(13) C(13) 117.0(11) . . 2_666
C(13) C(13) C(15) 119.1(8) 2_666 . .
C(11) C(14) C(15) 123.9(16) . . 2_666
C(13) C(15) C(14) 118.8(12) 2_666 2_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ni C(1) 1.868(5) . .
Ni C(2) 1.876(7) . .
Cd N(1) 2.373(5) . .
Cd N(3) 2.399(5) . .
Cd N(4) 2.352(5) . 1_554
C(1) N(1) 1.132(7) . .
C(2) N(2) 1.137(8) . .
N(3) C(3) 1.457(8) . .
C(3) C(4) 1.519(8) . .
C(4) C(5) 1.392(8) . .
C(5) C(6) 1.395(9) . .
C(6) C(7) 1.378(9) . .
C(7) C(8) 1.394(9) . .
C(8) C(9) 1.395(9) . .
C(9) C(4) 1.377(8) . .
C(7) C(10) 1.516(8) . .
N(4) C(10) 1.496(8) . .
N(11) C(11) 1.57(2) . .
C(11) C(12) 1.42(2) . .
C(12) C(13) 1.21(2) . .
C(13) C(13) 1.42(2) . 2_666
C(13) C(15) 1.48(1) . .
C(11) C(14) 1.41(2) . .
C(14) C(15) 1.20(2) . 2_666
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
N(2) N(3) 3.362(9) . 1_545
N(2) N(4) 3.093(10) . 1_544
N(2) N(11) 3.141(12) . 1_655