#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:31:53 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224277 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/90/7049046.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_7049046
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-2014
_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                   8.35570(10)
_cell_length_b                   8.35570(10)
_cell_length_c                   11.8796(3)
_cell_measurement_reflns_used    5809
_cell_measurement_temperature    140
_cell_measurement_theta_max      29.401
_cell_measurement_theta_min      3.448
_cell_volume                     829.41(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      140
_diffrn_detector_area_resol_mean 10.4508
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.946
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5809
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.401
_diffrn_reflns_theta_min         3.448
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.359
_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         0.461
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0470
_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)+(0.0126P)²+2.8245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                500
_reflns_number_total             575
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt05082a2.cif
_cod_data_source_block           bd231_a
_cod_depositor_comments
'Adding full bibliography for 7049046--7049047.cif.'
_cod_database_code               7049046
_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           2014-3
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
Cr1 Cr 0.5000 0.5000 1.0000 0.0140(3) Uani 1 8 d S T P
N1 N 0.6973(5) 0.8332(5) 1.0000 0.0539(14) Uani 1 2 d S T P
C1 C 0.6275(4) 0.7152(5) 1.0000 0.0217(8) Uani 1 2 d S T P
K1 K 0.5000 0.5000 0.5000 0.0162(3) Uani 1 8 d S T P
C2 C 0.5000 0.5000 0.8271(4) 0.0256(11) Uani 1 4 d S T P
N2 N 0.5000 0.5000 0.7293(4) 0.0495(17) Uani 1 4 d S T P
N1A N 0.5610(6) 0.9390(6) 0.7500 0.046(2) Uani 0.5 2 d S T P
H1A H 0.6062 0.8927 0.8110 0.055 Uiso 0.25 1 d R U P
H1B H 0.6062 0.8927 0.6890 0.055 Uiso 0.25 1 d R U P
C1A C 0.6016(5) 1.1016(5) 0.7500 0.0626(17) Uani 1 2 d S T P
H1AA H 0.7159 1.1131 0.7500 0.094 Uiso 0.5 1 d R U P
H1AB H 0.5578 1.1506 0.6840 0.094 Uiso 0.5 1 d R U P
H1AC H 0.5578 1.1506 0.8160 0.094 Uiso 0.5 1 d R U P
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_667 .
C2 Cr1 C1 90.000(1) 9_667 9_667
C2 Cr1 C1 90.000(1) . 9_667
C2 Cr1 C1 90.000(1) 9_667 11_567
C2 Cr1 C1 90.000(1) . 11_567
C1 Cr1 C1 90.0 9_667 11_567
C2 Cr1 C1 90.000(1) 9_667 3_655
C2 Cr1 C1 90.000(1) . 3_655
C1 Cr1 C1 90.000(1) 9_667 3_655
C1 Cr1 C1 180.0 11_567 3_655
C2 Cr1 C1 90.000(1) 9_667 .
C2 Cr1 C1 90.000(1) . .
C1 Cr1 C1 180.0 9_667 .
C1 Cr1 C1 90.000(1) 11_567 .
C1 Cr1 C1 90.000(1) 3_655 .
C1 N1 K1 149.5(3) . 5_656
N1 C1 Cr1 180.0(3) . .
N2 K1 N2 180.0 9_666 .
N2 K1 N1 90.000(1) 9_666 15_775
N2 K1 N1 90.000(1) . 15_775
N2 K1 N1 90.000(1) 9_666 7_446
N2 K1 N1 90.000(1) . 7_446
N1 K1 N1 180.0 15_775 7_446
N2 K1 N1 90.0 9_666 5_646
N2 K1 N1 90.0 . 5_646
N1 K1 N1 90.0 15_775 5_646
N1 K1 N1 90.0 7_446 5_646
N2 K1 N1 90.0 9_666 13_575
N2 K1 N1 90.0 . 13_575
N1 K1 N1 90.0 15_775 13_575
N1 K1 N1 90.000(1) 7_446 13_575
N1 K1 N1 180.0 5_646 13_575
N2 C2 Cr1 180.0 . .
C2 N2 K1 180.0 . .
C1A N1A C1A 118.0(5) 2_675 .
C1A N1A N1A 59.0(3) 2_675 2_675
C1A N1A N1A 59.0(3) . 2_675
C1A N1A H1A 107.5 2_675 .
C1A N1A H1A 108.3 . .
N1A N1A H1A 126.7 2_675 .
C1A N1A H1B 107.5 2_675 .
C1A N1A H1B 108.3 . .
N1A N1A H1B 126.7 2_675 .
H1A N1A H1B 106.6 . .
N1A C1A N1A 62.0(5) . 2_675
N1A C1A H1AA 109.7 . .
N1A C1A H1AA 171.7 2_675 .
N1A C1A H1AB 108.8 . .
N1A C1A H1AB 74.5 2_675 .
H1AA C1A H1AB 109.8 . .
N1A C1A H1AC 108.8 . .
N1A C1A H1AC 74.5 2_675 .
H1AA C1A H1AC 109.8 . .
H1AB C1A H1AC 110.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 C2 2.054(5) 9_667
Cr1 C2 2.054(5) .
Cr1 C1 2.090(4) 9_667
Cr1 C1 2.090(4) 11_567
Cr1 C1 2.090(4) 3_655
Cr1 C1 2.090(4) .
N1 C1 1.145(6) .
N1 K1 2.888(4) 5_656
K1 N2 2.724(5) 9_666
K1 N2 2.724(5) .
K1 N1 2.888(4) 15_775
K1 N1 2.888(4) 7_446
K1 N1 2.888(4) 5_646
K1 N1 2.888(4) 13_575
C2 N2 1.162(7) .
N1A C1A 1.401(6) 2_675
N1A C1A 1.401(6) .
N1A N1A 1.442(13) 2_675
N1A H1A 0.9039 .
N1A H1B 0.9039 .
C1A N1A 1.401(6) 2_675
C1A H1AA 0.9593 .
C1A H1AB 0.9571 .
C1A H1AC 0.9571 .
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
N1A H1A N1 0.90 2.42 3.301(3) 164.2 .
N1A H1B N1 0.90 2.42 3.301(3) 164.5 15_775
C1A H1AA N2 0.96 2.57 3.444(3) 152.1 5_656
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
C1A N1A C1A N1A 0.0 2_675 2_675
