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#$Date: 2017-04-21 07:32:37 +0300 (Fri, 21 Apr 2017) $
#$Revision: 195650 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/80/7228097.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_7228097
loop_
_publ_author_name
'Ptak, Maciej'
'Gągor, Anna'
'Sieradzki, Adam'
'Bondzior, Bartosz'
'Dereń, Przemysław Jacek'
'Ciupa, Aneta'
'Trzebiatowska, Monika'
'Maczka, Miroslaw'
_publ_section_title
;
 Effect of K+ cations on phase transitions, structural, dielectric and
 luminescent properties of [cat][K0.5Cr0.5(HCOO)3], where cat is
 protonated dimethylamine or ethylamine
;
_journal_name_full               'Phys. Chem. Chem. Phys.'
_journal_paper_doi               10.1039/C7CP01336A
_journal_year                    2017
_chemical_formula_sum            'C10 H22 Cr K N2 O12'
_chemical_formula_weight         453.39
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-06 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   8.5676(2)
_cell_length_b                   8.5676(2)
_cell_length_c                   23.7293(9)
_cell_measurement_reflns_used    2348
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.9440
_cell_measurement_theta_min      2.5670
_cell_volume                     1508.46(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.4350
_diffrn_detector_type            'Sapphire1, long nozzle'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            4856
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.609
_diffrn_reflns_theta_max         25.609
_diffrn_reflns_theta_min         2.575
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       prism
_exptl_crystal_F_000             705
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0304
_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)+(0.0284P)²+1.9592P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                573
_reflns_number_total             641
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cp01336a2.cif
_cod_data_source_block           DMAKCr
_cod_original_cell_volume        1508.46(9)
_cod_database_code               7228097
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
C2 C 0.645(3) 0.305(2) 0.0412(2) 0.061(2) Uiso 0.3333 1 d . . P
H2A H 0.7544 0.4109 0.0303 0.092 Uiso 0.3333 1 calc R U P
H2B H 0.5512 0.2833 0.0148 0.092 Uiso 0.3333 1 calc R U P
H2C H 0.6636 0.2031 0.0413 0.092 Uiso 0.3333 1 calc R U P
N1 N 0.5957(8) 0.3282(9) 0.0940(2) 0.0545(15) Uiso 0.3333 1 d . . P
H1A H 0.6266 0.4440 0.0949 0.065 Uiso 0.3333 1 calc R U P
H1B H 0.4757 0.2672 0.0932 0.065 Uiso 0.3333 1 calc R U P
C3 C 0.636(7) 0.297(9) 0.1434(3) 0.089(9) Uani 0.3333 1 d . . P
H3A H 0.6737 0.2097 0.1409 0.133 Uiso 0.3333 1 calc R U P
H3B H 0.5315 0.2523 0.1673 0.133 Uiso 0.3333 1 calc R U P
H3C H 0.7312 0.4072 0.1589 0.133 Uiso 0.3333 1 calc R U P
Cr1 Cr 1.0000 1.0000 0.0000 0.0348(2) Uani 1 6 d S T P
K1 K 0.3333 0.6667 0.1667 0.0391(3) Uani 1 6 d S T P
O1 O 0.82710(19) 0.79783(19) 0.04735(6) 0.0465(4) Uani 1 1 d . . .
C1 C 0.6873(3) 0.7819(3) 0.07052(9) 0.0518(6) Uani 1 1 d . . .
H1 H 0.6638 0.8760 0.0657 0.062 Uiso 1 1 calc R U .
O2 O 0.5805(3) 0.6535(3) 0.09865(9) 0.0847(7) Uani 1 1 d . . .
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'
O O 0.0106 0.0060 '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
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C3 N1 C2 132(5) . .
C3 N1 H1A 104.2 . .
C2 N1 H1A 104.2 . .
C3 N1 H1B 104.2 . .
C2 N1 H1B 104.2 . .
H1A N1 H1B 105.5 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
O1 Cr1 O1 180.00(11) 11_565 2_765
O1 Cr1 O1 90.76(6) 11_565 12_655
O1 Cr1 O1 89.24(6) 2_765 12_655
O1 Cr1 O1 89.24(6) 11_565 3_675
O1 Cr1 O1 90.76(6) 2_765 3_675
O1 Cr1 O1 180.00(7) 12_655 3_675
O1 Cr1 O1 90.76(6) 11_565 10_775
O1 Cr1 O1 89.24(6) 2_765 10_775
O1 Cr1 O1 90.76(6) 12_655 10_775
O1 Cr1 O1 89.24(6) 3_675 10_775
O1 Cr1 O1 89.24(6) 11_565 .
O1 Cr1 O1 90.76(6) 2_765 .
O1 Cr1 O1 89.24(6) 12_655 .
O1 Cr1 O1 90.76(6) 3_675 .
O1 Cr1 O1 180.0 10_775 .
O2 K1 O2 88.15(7) . 3_565
O2 K1 O2 88.15(7) . 2_665
O2 K1 O2 88.14(7) 3_565 2_665
O2 K1 O2 91.86(7) . 14_455
O2 K1 O2 91.86(7) 3_565 14_455
O2 K1 O2 180.0 2_665 14_455
O2 K1 O2 91.86(7) . 15
O2 K1 O2 180.0 3_565 15
O2 K1 O2 91.85(7) 2_665 15
O2 K1 O2 88.14(7) 14_455 15
O2 K1 O2 180.0 . 13_565
O2 K1 O2 91.85(7) 3_565 13_565
O2 K1 O2 91.85(7) 2_665 13_565
O2 K1 O2 88.14(7) 14_455 13_565
O2 K1 O2 88.14(7) 15 13_565
O2 K1 C1 16.98(5) . .
O2 K1 C1 95.18(6) 3_565 .
O2 K1 C1 72.98(6) 2_665 .
O2 K1 C1 107.02(6) 14_455 .
O2 K1 C1 84.83(6) 15 .
O2 K1 C1 163.02(6) 13_565 .
O2 K1 C1 95.18(6) . 2_665
O2 K1 C1 72.98(6) 3_565 2_665
O2 K1 C1 16.98(6) 2_665 2_665
O2 K1 C1 163.02(6) 14_455 2_665
O2 K1 C1 107.02(6) 15 2_665
O2 K1 C1 84.82(6) 13_565 2_665
C1 K1 C1 82.49(6) . 2_665
O2 K1 C1 72.98(6) . 3_565
O2 K1 C1 16.99(5) 3_565 3_565
O2 K1 C1 95.18(6) 2_665 3_565
O2 K1 C1 84.83(6) 14_455 3_565
O2 K1 C1 163.02(6) 15 3_565
O2 K1 C1 107.02(6) 13_565 3_565
C1 K1 C1 82.50(6) . 3_565
C1 K1 C1 82.49(6) 2_665 3_565
O2 K1 C1 84.82(6) . 14_455
O2 K1 C1 107.02(6) 3_565 14_455
O2 K1 C1 163.02(6) 2_665 14_455
O2 K1 C1 16.98(6) 14_455 14_455
O2 K1 C1 72.98(6) 15 14_455
O2 K1 C1 95.17(6) 13_565 14_455
C1 K1 C1 97.51(6) . 14_455
C1 K1 C1 180.0 2_665 14_455
C1 K1 C1 97.51(6) 3_565 14_455
O2 K1 C1 107.02(6) . 15
O2 K1 C1 163.01(6) 3_565 15
O2 K1 C1 84.82(6) 2_665 15
O2 K1 C1 95.17(6) 14_455 15
O2 K1 C1 16.98(5) 15 15
O2 K1 C1 72.98(6) 13_565 15
C1 K1 C1 97.51(6) . 15
C1 K1 C1 97.51(6) 2_665 15
C1 K1 C1 180.0 3_565 15
C1 K1 C1 82.49(6) 14_455 15
O2 K1 C1 163.02(6) . 13_565
O2 K1 C1 84.82(6) 3_565 13_565
O2 K1 C1 107.02(6) 2_665 13_565
O2 K1 C1 72.98(6) 14_455 13_565
O2 K1 C1 95.17(6) 15 13_565
O2 K1 C1 16.98(5) 13_565 13_565
C1 K1 C1 180.0 . 13_565
C1 K1 C1 97.51(6) 2_665 13_565
C1 K1 C1 97.51(6) 3_565 13_565
C1 K1 C1 82.49(6) 14_455 13_565
C1 K1 C1 82.49(6) 15 13_565
C1 O1 Cr1 126.75(15) . .
O2 C1 O1 125.4(2) . .
O1 C1 K1 162.00(16) . .
O2 C1 H1 117.3 . .
O1 C1 H1 117.3 . .
K1 C1 H1 78.0 . .
C1 O2 K1 122.55(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C2 N1 1.370(15) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
N1 C3 1.29(4) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
Cr1 O1 1.9726(14) 11_565
Cr1 O1 1.9726(14) 2_765
Cr1 O1 1.9726(14) 12_655
Cr1 O1 1.9726(14) 3_675
Cr1 O1 1.9726(14) 10_775
Cr1 O1 1.9726(14) .
K1 O2 2.7092(18) .
K1 O2 2.7092(18) 3_565
K1 O2 2.7092(18) 2_665
K1 O2 2.7092(18) 14_455
K1 O2 2.7092(18) 15
K1 O2 2.7093(18) 13_565
K1 C1 3.519(2) .
K1 C1 3.519(2) 2_665
K1 C1 3.519(2) 3_565
K1 C1 3.519(2) 14_455
K1 C1 3.519(2) 15
K1 C1 3.519(2) 13_565
O1 C1 1.262(3) .
C1 O2 1.219(3) .
C1 H1 0.9300 .
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
N1 H1A O2 0.89 2.02 2.856(7) 155.3 .
N1 H1B O1 0.89 2.46 3.243(6) 146.8 2_655
N1 H1B O2 0.89 2.55 3.008(7) 112.6 2_655
