#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:51:35 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178966 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/95/4119559.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_4119559
loop_
_publ_author_name
'Wen Zhang'
'Heng-Yun Ye'
'Robert Graf'
'Hans W. Spiess'
'Ye-Feng Yao'
'Run-Qiang Zhu'
'Ren-Gen Xiong'
_publ_section_title
;
 Tunable and Switchable Dielectric Constant in an Amphidynamic Crystal
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5230
_journal_page_last               5233
_journal_paper_doi               10.1021/ja3110335
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C10 H12 Co D4 K N8'
_chemical_formula_weight         350.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           128
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_atom_sites_solution_hydrogens   ..
_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            2
_cell_length_a                   8.277(5)
_cell_length_b                   8.277(5)
_cell_length_c                   11.622(9)
_cell_measurement_reflns_used    1818
_cell_measurement_temperature    280(2)
_cell_measurement_theta_max      27.4468
_cell_measurement_theta_min      3.0207
_cell_volume                     796.2(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      280(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7669
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8994
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    ..
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0487
_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)+(0.0517P)²+0.8960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                473
_reflns_number_total             484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3110335_si_002_4.cif
_cod_data_source_block           2-280K
_cod_original_cell_volume        796.1(9)
_cod_database_code               4119559
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, 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_group
Co1 Co 0.0000 1.0000 0.0000 0.0215(3) Uani 1 8 d S .
K1 K 0.5000 0.5000 0.0000 0.0290(4) Uani 1 8 d S .
C1 C 0.1897(5) 0.8710(5) 0.0000 0.0387(9) Uani 1 2 d S .
C2 C 0.0000 1.0000 0.1626(5) 0.0492(17) Uani 1 4 d S .
N1 N 0.3060(7) 0.7981(7) 0.0000 0.0741(16) Uani 1 2 d S .
N2 N 0.5000 0.5000 0.2392(5) 0.089(4) Uani 1 4 d S .
C3 C 0.3995(8) 0.1005(8) 0.2500 0.107(3) Uani 0.59(3) 2 d SP 1
H3A H 0.3867(8) 0.2180(8) 0.2500 0.160 Uiso 0.297(17) 1 d PR 1
H3B H 0.3495(8) 0.0585(8) 0.1825 0.160 Uiso 0.297(17) 1 d PR 1
H3C H 0.3495(8) 0.0585(8) 0.3175 0.160 Uiso 0.297(17) 1 d PR 1
N3 N 0.5650(13) 0.0650(13) 0.2500 0.050(6) Uani 0.297(17) 2 d SP 1
D1 D 0.6105 0.1095 0.3124 0.060 Uiso 0.297(17) 1 d PR 1
C3' C 0.3995(8) 0.1005(8) 0.2500 0.107(3) Uani 0.41(3) 2 d SP 2
H3'A H 0.334(3) 0.167(3) 0.1989 0.160 Uiso 0.203(17) 1 d PR 2
H3'B H 0.329(3) 0.039(3) 0.2976 0.160 Uiso 0.203(17) 1 d PR 2
H3'C H 0.463(3) 0.172(3) 0.2976 0.160 Uiso 0.203(17) 1 d PR 2
N3' N 0.5000 0.0000 0.181(3) 0.069(10) Uani 0.203(17) 2 d SP 2
D1' D 0.5619 0.0619 0.1353 0.082 Uiso 0.203(17) 1 d PR 2
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 '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
C2 Co1 C2 180.000(1) 9_575 .
C2 Co1 C1 90.0 9_575 11_465
C2 Co1 C1 90.0 . 11_465
C2 Co1 C1 90.0 9_575 3_665
C2 Co1 C1 90.0 . 3_665
C1 Co1 C1 180.000(1) 11_465 3_665
C2 Co1 C1 90.000(1) 9_575 .
C2 Co1 C1 90.000(1) . .
C1 Co1 C1 90.0 11_465 .
C1 Co1 C1 90.0 3_665 .
C2 Co1 C1 90.000(1) 9_575 9_575
C2 Co1 C1 90.000(1) . 9_575
C1 Co1 C1 90.0 11_465 9_575
C1 Co1 C1 90.000(1) 3_665 9_575
C1 Co1 C1 180.0 . 9_575
N2 K1 N2 180.0 9_665 .
N2 K1 N1 90.0 9_665 3_655
N2 K1 N1 90.0 . 3_655
N2 K1 N1 90.0 9_665 11_565
N2 K1 N1 90.0 . 11_565
N1 K1 N1 180.0 3_655 11_565
N2 K1 N1 90.0 9_665 .
N2 K1 N1 90.0 . .
N1 K1 N1 90.0 3_655 .
N1 K1 N1 90.0 11_565 .
N2 K1 N1 90.0 9_665 9_665
N2 K1 N1 90.0 . 9_665
N1 K1 N1 90.0 3_655 9_665
N1 K1 N1 90.0 11_565 9_665
N1 K1 N1 180.0 . 9_665
N1 C1 Co1 177.9(5) . .
N2 C2 Co1 180.000(1) 5 .
C1 N1 K1 155.1(5) . .
C2 N2 K1 180.000(1) 5_545 .
H3B C3 H3B 174.3 8 .
H3B C3 H3C 68.8 8 .
H3B C3 H3C 110.9 . .
H3B C3 H3C 110.9 8 8
H3B C3 H3C 68.8 . 8
H3C C3 H3C 174.3 . 8
H3B C3 H3A 108.4 8 8
H3B C3 H3A 66.9 . 8
H3C C3 H3A 66.9 . 8
H3C C3 H3A 108.4 8 8
H3B C3 H3A 66.9 8 .
H3B C3 H3A 108.4 . .
H3C C3 H3A 108.4 . .
H3C C3 H3A 66.9 8 .
H3A C3 H3A 77.6 8 .
H3B C3 N3 110.4(3) 8 2_655
H3B C3 N3 74.6(3) . 2_655
H3C C3 N3 74.6(3) . 2_655
H3C C3 N3 110.4(3) 8 2_655
H3A C3 N3 108.3(6) 8 2_655
H3A C3 N3 174.1(6) . 2_655
H3B C3 N3 74.6(3) 8 .
H3B C3 N3 110.4(3) . .
H3C C3 N3 110.4(3) . .
H3C C3 N3 74.6(3) 8 .
H3A C3 N3 174.1(6) 8 .
H3A C3 N3 108.3(6) . .
N3 C3 N3 65.8(11) 2_655 .
C3 H3A H3B 55.3 . 8
C3 H3A H3C 55.3 . 8
H3B H3A H3C 94.9 8 8
C3 H3B H3A 57.8 . 8
C3 H3B H3C 55.6 . 8
H3A H3B H3C 94.1 8 8
C3 H3B N3 66.8(4) . 2_655
H3A H3B N3 99.0(2) 8 2_655
H3C H3B N3 98.7(6) 8 2_655
C3 H3C H3A 57.8 . 8
C3 H3C H3B 55.6 . 8
H3A H3C H3B 94.1 8 8
C3 H3C N3 66.8(4) . 2_655
H3A H3C N3 99.0(2) 8 2_655
H3B H3C N3 98.7(6) 8 2_655
C3 N3 C3 114.2(11) 2_655 .
C3 N3 H3B 38.6(2) 2_655 2_655
C3 N3 H3B 128.0(9) . 2_655
C3 N3 H3C 128.0(9) 2_655 8
C3 N3 H3C 38.6(2) . 8
H3B N3 H3C 112.6(5) 2_655 8
C3 N3 H3B 128.0(9) 2_655 8
C3 N3 H3B 38.6(2) . 8
H3B N3 H3B 162.5(11) 2_655 8
H3C N3 H3B 64.5(4) 8 8
C3 N3 H3C 38.6(2) 2_655 2_655
C3 N3 H3C 128.0(9) . 2_655
H3B N3 H3C 64.5(4) 2_655 2_655
H3C N3 H3C 162.5(11) 8 2_655
H3B N3 H3C 112.6(5) 8 2_655
C3 N3 N3 57.1(6) 2_655 2_655
C3 N3 N3 57.1(6) . 2_655
H3B N3 N3 81.3(6) 2_655 2_655
H3C N3 N3 81.3(6) 8 2_655
H3B N3 N3 81.3(6) 8 2_655
H3C N3 N3 81.3(6) 2_655 2_655
H3'B H3'A H3'C 94.3 8 8
H3'A H3'B H3'C 92.6 8 8
H3'A H3'B N3' 100.4(6) 8 7_545
H3'C H3'B N3' 100.0(10) 8 7_545
H3'A H3'C H3'B 91.7 8 8
H3'A H3'C N3' 99.2(6) 8 7_545
H3'B H3'C N3' 99.3(10) 8 7_545
C3' N3' H3'B 126.4(13) 2_655 8
C3' N3' H3'B 38.5(6) 2_655 7_545
H3'B N3' H3'B 161(2) 8 7_545
C3' N3' H3'C 38.8(6) 2_655 7_545
H3'B N3' H3'C 112.5(7) 8 7_545
H3'B N3' H3'C 64.0(15) 7_545 7_545
C3' N3' H3'C 126.3(13) 2_655 8
H3'B N3' H3'C 64.0(15) 8 8
H3'B N3' H3'C 112.5(7) 7_545 8
H3'C N3' H3'C 161(2) 7_545 8
C3' N3' N3' 55.7(11) 2_655 7_545
H3'B N3' N3' 80.3(10) 8 7_545
H3'B N3' N3' 80.3(10) 7_545 7_545
H3'C N3' N3' 80.4(10) 7_545 7_545
H3'C N3' N3' 80.4(10) 8 7_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 C2 1.890(6) 9_575
Co1 C2 1.890(6) .
Co1 C1 1.899(4) 11_465
Co1 C1 1.899(4) 3_665
Co1 C1 1.899(4) .
Co1 C1 1.899(4) 9_575
K1 N2 2.780(6) 9_665
K1 N2 2.780(6) .
K1 N1 2.944(5) 3_655
K1 N1 2.944(5) 11_565
K1 N1 2.944(5) .
K1 N1 2.944(5) 9_665
C1 N1 1.135(6) .
C2 N2 1.141(8) 5
N2 C2 1.141(8) 5_545
C3 H3B 0.9519 8
C3 H3B 0.9519 .
C3 H3C 0.9519 .
C3 H3C 0.9519 8
C3 H3A 0.9789 8
C3 H3A 0.9789 .
C3 N3 1.401(11) 2_655
C3 N3 1.401(11) .
H3A H3B 1.0643 8
H3A H3C 1.0643 8
H3B H3A 1.0643 8
H3B H3C 1.0759 8
H3B N3 1.470(8) 2_655
H3C H3A 1.0643 8
H3C H3B 1.0759 8
H3C N3 1.470(8) 2_655
N3 C3 1.401(11) 2_655
N3 H3B 1.470(8) 2_655
N3 H3C 1.470(8) 8
N3 H3B 1.470(8) 8
N3 H3C 1.470(8) 2_655
N3 N3 1.52(3) 2_655
H3'A H3'B 1.0588 8
H3'A H3'C 1.0762 8
H3'B H3'A 1.0588 8
H3'B H3'C 1.1072 8
H3'B N3' 1.47(3) 7_545
H3'C H3'A 1.0762 8
H3'C H3'B 1.1072 8
H3'C N3' 1.48(3) 7_545
N3' C3' 1.423(17) 2_655
N3' H3'B 1.47(3) 8
N3' H3'B 1.47(3) 7_545
N3' H3'C 1.48(3) 7_545
N3' H3'C 1.48(3) 8
N3' N3' 1.60(6) 7_545
