#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:31:53 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224277 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/90/7049047.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_7049047
loop_
_publ_author_name
'Rok, M.'
'Bator, G.'
'Zarychta, B.'
'Dziuk, B.'
'Repeć, J'
'Medycki, W.'
'Zamponi, M.'
'Usevičius, G'
'Šimėnas, M'
'Banys, J.'
_publ_section_title
;
 Isostructural phase transition, quasielastic neutron scattering and
 magnetic resonance studies of a bistable dielectric ion-pair crystal
 [(CH₃)₂NH₂]₂KCr(CN)₆.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4190
_journal_page_last               4202
_journal_paper_doi               10.1039/c8dt05082a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C6 Cr K N6, 2(C2 H8 N)'
_chemical_formula_sum            'C10 H16 Cr K N8'
_chemical_formula_weight         339.41
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-11-16 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.40300(10)
_cell_length_b                   8.40300(10)
_cell_length_c                   11.8999(3)
_cell_measurement_reflns_used    6061
_cell_measurement_temperature    230
_cell_measurement_theta_max      29.508
_cell_measurement_theta_min      3.424
_cell_volume                     840.26(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      230
_diffrn_detector_area_resol_mean 10.4508
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device       '4-circle kappa geometry goniometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur System'
_diffrn_measurement_method       ω--scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6061
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.508
_diffrn_reflns_theta_min         3.424
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             350
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0096(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         597
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0312P)²+0.0902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                446
_reflns_number_total             597
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt05082a2.cif
_cod_data_source_block           bd230_a
_cod_depositor_comments
'Adding full bibliography for 7049046--7049047.cif.'
_cod_database_code               7049047
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.5000 0.5000 0.0000 0.02301(17) Uani 1 8 d S T P . .
K1 K 0.5000 0.5000 0.5000 0.02818(18) Uani 1 8 d S T P . .
C1 C 0.2893(2) 0.3699(2) 0.0000 0.0364(4) Uani 1 2 d S T P . .
N1 N 0.1733(2) 0.2998(2) 0.0000 0.0687(6) Uani 1 2 d S T P . .
C2 C 0.5000 0.5000 0.1731(2) 0.0444(7) Uani 1 4 d S T P . .
N2 N 0.5000 0.5000 0.2690(2) 0.0858(13) Uani 1 4 d S T P . .
C1A C 0.4002(3) 0.0998(3) 0.2500 0.1010(11) Uani 1 2 d S TU P A 1
H1AC H 0.2866 0.1125 0.2500 0.151 Uiso 0.5 1 d R U P A 1
H1AD H 0.4437 0.1504 0.3159 0.151 Uiso 0.5 1 d R U P A 1
H1AE H 0.4437 0.1504 0.1841 0.151 Uiso 0.5 1 d R U P A 1
N1AA N 0.4377(6) -0.0623(6) 0.2500 0.0558(15) Uani 0.3 2 d S TU P A 1
H1AA H 0.3928 -0.1065 0.1891 0.067 Uiso 0.15 1 d R U P A 1
H1AB H 0.3928 -0.1065 0.3109 0.067 Uiso 0.15 1 d R U P A 1
N1AB N 0.5000 0.0000 0.1851(12) 0.095(4) Uani 0.2 2 d S TU P B 2
H1AF H 0.5610 0.0611 0.1403 0.114 Uiso 0.1 1 d R U P B 2
H1AG H 0.4390 -0.0611 0.1403 0.114 Uiso 0.1 1 d R U P B 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'
Cr Cr 0.3209 0.6236 '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 Cr1 C2 180.0 9_665 .
C2 Cr1 C1 90.0 9_665 9_665
C2 Cr1 C1 90.0 . 9_665
C2 Cr1 C1 90.0 9_665 11_565
C2 Cr1 C1 90.0 . 11_565
C1 Cr1 C1 90.0 9_665 11_565
C2 Cr1 C1 90.0 9_665 3_655
C2 Cr1 C1 90.0 . 3_655
C1 Cr1 C1 90.0 9_665 3_655
C1 Cr1 C1 180.0 11_565 3_655
C2 Cr1 C1 90.0 9_665 .
C2 Cr1 C1 90.0 . .
C1 Cr1 C1 180.0 9_665 .
C1 Cr1 C1 90.0 11_565 .
C1 Cr1 C1 90.0 3_655 .
N2 K1 N2 180.0 9_666 .
N2 K1 N1 90.0 9_666 15_666
N2 K1 N1 90.0 . 15_666
N2 K1 N1 90.0 9_666 7
N2 K1 N1 90.0 . 7
N1 K1 N1 180.00(6) 15_666 7
N2 K1 N1 90.0 9_666 5
N2 K1 N1 90.0 . 5
N1 K1 N1 90.0 15_666 5
N1 K1 N1 90.0 7 5
N2 K1 N1 90.0 9_666 13_666
N2 K1 N1 90.0 . 13_666
N1 K1 N1 90.0 15_666 13_666
N1 K1 N1 90.0 7 13_666
N1 K1 N1 180.0 5 13_666
N1 C1 Cr1 179.45(17) . .
C1 N1 K1 151.16(16) . 5_545
N2 C2 Cr1 180.0 . .
C2 N2 K1 180.0 . .
N1AA C1A N1AA 64.0(5) 2_655 .
N1AA C1A H1AC 173.4 2_655 .
N1AA C1A H1AC 109.4 . .
N1AA C1A H1AD 74.4 2_655 .
N1AA C1A H1AD 110.2 . .
H1AC C1A H1AD 109.1 . .
N1AA C1A H1AE 74.4 2_655 .
N1AA C1A H1AE 110.2 . .
H1AC C1A H1AE 109.1 . .
H1AD C1A H1AE 108.9 . .
C1A N1AA C1A 116.0(5) 2_655 .
C1A N1AA N1AA 58.0(3) 2_655 2_655
C1A N1AA N1AA 58.0(3) . 2_655
C1A N1AA H1AA 108.4 2_655 .
C1A N1AA H1AA 108.0 . .
N1AA N1AA H1AA 126.2 2_655 .
C1A N1AA H1AB 108.4 2_655 .
C1A N1AA H1AB 108.0 . .
N1AA N1AA H1AB 126.2 2_655 .
H1AA N1AA H1AB 107.7 . .
N1AB N1AB H1AF 126.3 7_545 .
N1AB N1AB H1AG 126.3 7_545 .
H1AF N1AB H1AG 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 C2 2.060(3) 9_665
Cr1 C2 2.060(3) .
Cr1 C1 2.0805(17) 9_665
Cr1 C1 2.0805(17) 11_565
Cr1 C1 2.0805(17) 3_655
Cr1 C1 2.0806(17) .
K1 N2 2.749(3) 9_666
K1 N2 2.749(3) .
K1 N1 2.9100(17) 15_666
K1 N1 2.9100(17) 7
K1 N1 2.9100(16) 5
K1 N1 2.9100(16) 13_666
C1 N1 1.139(2) .
N1 K1 2.9100(16) 5_545
C2 N2 1.141(3) .
C1A N1AA 1.398(5) 2_655
C1A N1AA 1.398(5) .
C1A H1AC 0.9609 .
C1A H1AD 0.9637 .
C1A H1AE 0.9637 .
N1AA C1A 1.398(5) 2_655
N1AA N1AA 1.481(14) 2_655
N1AA H1AA 0.8975 .
N1AA H1AB 0.8975 .
N1AB N1AB 1.55(3) 7_545
N1AB H1AF 0.9000 .
N1AB H1AG 0.9000 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1A H1AC N2 0.96 2.60 3.4735(19) 151.7 5_545
N1AA H1AA N1 0.90 2.45 3.326(3) 166.3 11
N1AA H1AB N1 0.90 2.45 3.326(3) 166.1 5_545
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1AA C1A N1AA C1A 0.0 2_655 2_655
