#------------------------------------------------------------------------------
#$Date: 2019-03-30 04:26:39 +0200 (Sat, 30 Mar 2019) $
#$Revision: 214424 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/25/7232553.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_7232553
loop_
_publ_author_name
'Ptak, Maciej'
'Dziuk, Błażej'
'Stefańska, Dagmara'
'Hermanowicz, Krzysztof'
_publ_section_title
;
 The structural, phonon and optical properties of
 [CH3NH3]M0.5CrxAl0.5−x(HCOO)3 (M = Na, K; x = 0, 0.025, 0.5)
 metal--organic framework perovskites for luminescence thermometry
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/C9CP01043B
_journal_year                    2019
_chemical_formula_sum            'C8 H18 Cr K N2 O12'
_chemical_formula_weight         425.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-05 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.410(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1907(5)
_cell_length_b                   9.0549(7)
_cell_length_c                   12.2909(8)
_cell_measurement_reflns_used    5936
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      25.997
_cell_measurement_theta_min      2.999
_cell_volume                     911.54(11)
_computing_cell_refinement       'CrysAlisCCD (Oxford Diffraction Ltd., 2008)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction Ltd., 2008)'
_computing_data_reduction        'CrysAlisCCD (Oxford Diffraction Ltd., 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean '1024 x 1024 with blocks 2 x 2'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       ω--scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.1032
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       5
_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       -15
_diffrn_reflns_number            5936
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.999
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'slightly purple'
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0439
_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)+(0.0278P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                992
_reflns_number_total             1779
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cp01043b2.cif
_cod_data_source_block           100K_CCDC1
_cod_database_code               7232553
_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'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-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 0.5000 0.0118(2) Uani 1 2 d S . P
O1 O 0.6309(3) 0.5323(3) 0.36832(18) 0.0132(6) Uani 1 1 d . . .
C1 C 0.5808(4) 0.5155(4) 0.2714(3) 0.0201(9) Uani 1 1 d . . .
H1 H 0.4746 0.4818 0.2610 0.024 Uiso 1 1 calc R U .
K1 K 0.0000 0.0000 0.5000 0.0195(3) Uani 1 2 d S . P
N1 N 0.5013(4) 0.0493(3) 0.2578(3) 0.0188(8) Uani 1 1 d . . .
H1A H 0.4744 0.1026 0.1995 0.028 Uiso 1 1 calc R U .
H1B H 0.6069 0.0614 0.2726 0.028 Uiso 1 1 calc R U .
H1C H 0.4425 0.0788 0.3143 0.028 Uiso 1 1 calc R U .
O3 O 0.4419(3) 0.3038(3) 0.4435(2) 0.0146(6) Uani 1 1 d . . .
C3 C 0.2172(5) 0.6845(4) 0.4624(3) 0.0213(10) Uani 1 1 d . . .
H3 H 0.2549 0.7335 0.5242 0.026 Uiso 1 1 calc R U .
C2 C 0.3119(5) 0.2330(5) 0.4637(3) 0.0234(10) Uani 1 1 d . . .
H2 H 0.2393 0.2731 0.5134 0.028 Uiso 1 1 calc R U .
O2 O 0.6630(3) 0.5406(3) 0.1898(2) 0.0254(7) Uani 1 1 d . . .
C4 C 0.4682(5) -0.1083(5) 0.2359(4) 0.0353(13) Uani 1 1 d . . .
H4A H 0.3543 -0.1212 0.2195 0.053 Uiso 1 1 calc R U .
H4B H 0.4968 -0.1657 0.2988 0.053 Uiso 1 1 calc R U .
H4C H 0.5320 -0.1403 0.1750 0.053 Uiso 1 1 calc R U .
O4 O 0.2765(3) 0.1139(3) 0.4210(2) 0.0284(8) Uani 1 1 d . . .
O6 O 0.0877(3) 0.7275(3) 0.4226(2) 0.0273(7) Uani 1 1 d . . .
O5 O 0.3036(3) 0.5799(3) 0.4272(2) 0.0152(6) 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'
O O 0.0106 0.0060 '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
O3 Cr1 O3 180.0 3_666 .
O3 Cr1 O1 88.60(9) 3_666 3_666
O3 Cr1 O1 91.40(9) . 3_666
O3 Cr1 O1 91.40(9) 3_666 .
O3 Cr1 O1 88.60(9) . .
O1 Cr1 O1 180.0 3_666 .
O3 Cr1 O5 88.65(10) 3_666 3_666
O3 Cr1 O5 91.35(10) . 3_666
O1 Cr1 O5 91.12(10) 3_666 3_666
O1 Cr1 O5 88.88(10) . 3_666
O3 Cr1 O5 91.35(10) 3_666 .
O3 Cr1 O5 88.65(10) . .
O1 Cr1 O5 88.88(10) 3_666 .
O1 Cr1 O5 91.12(10) . .
O5 Cr1 O5 180.0 3_666 .
C1 O1 Cr1 125.5(2) . .
O2 C1 O1 124.6(3) . .
O2 C1 K1 46.61(18) . 2
O1 C1 K1 171.0(3) . 2
O2 C1 H1 117.7 . .
O1 C1 H1 117.7 . .
K1 C1 H1 71.1 2 .
O4 K1 O4 180.0 . 3_556
O4 K1 O2 87.23(8) . 4_566
O4 K1 O2 92.77(8) 3_556 4_566
O4 K1 O2 92.77(8) . 2_545
O4 K1 O2 87.23(8) 3_556 2_545
O2 K1 O2 180.0 4_566 2_545
O4 K1 O6 90.20(8) . 3_566
O4 K1 O6 89.80(8) 3_556 3_566
O2 K1 O6 87.24(8) 4_566 3_566
O2 K1 O6 92.76(8) 2_545 3_566
O4 K1 O6 89.80(8) . 1_545
O4 K1 O6 90.20(8) 3_556 1_545
O2 K1 O6 92.76(8) 4_566 1_545
O2 K1 O6 87.24(8) 2_545 1_545
O6 K1 O6 180.0 3_566 1_545
O4 K1 C2 19.92(8) . .
O4 K1 C2 160.08(8) 3_556 .
O2 K1 C2 80.11(9) 4_566 .
O2 K1 C2 99.89(9) 2_545 .
O6 K1 C2 71.40(9) 3_566 .
O6 K1 C2 108.60(9) 1_545 .
O4 K1 C2 160.07(8) . 3_556
O4 K1 C2 19.93(8) 3_556 3_556
O2 K1 C2 99.89(9) 4_566 3_556
O2 K1 C2 80.11(9) 2_545 3_556
O6 K1 C2 108.60(9) 3_566 3_556
O6 K1 C2 71.40(9) 1_545 3_556
C2 K1 C2 180.0 . 3_556
O4 K1 C1 102.26(9) . 4_566
O4 K1 C1 77.74(9) 3_556 4_566
O2 K1 C1 19.33(7) 4_566 4_566
O2 K1 C1 160.67(7) 2_545 4_566
O6 K1 C1 75.30(9) 3_566 4_566
O6 K1 C1 104.70(9) 1_545 4_566
C2 K1 C1 90.76(10) . 4_566
C2 K1 C1 89.24(10) 3_556 4_566
O4 K1 C1 77.74(9) . 2_545
O4 K1 C1 102.26(9) 3_556 2_545
O2 K1 C1 160.67(7) 4_566 2_545
O2 K1 C1 19.33(7) 2_545 2_545
O6 K1 C1 104.70(9) 3_566 2_545
O6 K1 C1 75.30(9) 1_545 2_545
C2 K1 C1 89.24(10) . 2_545
C2 K1 C1 90.76(10) 3_556 2_545
C1 K1 C1 180.0 4_566 2_545
O4 K1 C3 80.19(9) . 1_545
O4 K1 C3 99.81(9) 3_556 1_545
O2 K1 C3 75.37(9) 4_566 1_545
O2 K1 C3 104.63(9) 2_545 1_545
O6 K1 C3 160.42(8) 3_566 1_545
O6 K1 C3 19.58(8) 1_545 1_545
C2 K1 C3 96.37(10) . 1_545
C2 K1 C3 83.63(10) 3_556 1_545
C1 K1 C3 90.01(10) 4_566 1_545
C1 K1 C3 89.99(10) 2_545 1_545
O4 K1 C3 99.81(9) . 3_566
O4 K1 C3 80.19(9) 3_556 3_566
O2 K1 C3 104.63(9) 4_566 3_566
O2 K1 C3 75.37(9) 2_545 3_566
O6 K1 C3 19.58(8) 3_566 3_566
O6 K1 C3 160.42(8) 1_545 3_566
C2 K1 C3 83.63(10) . 3_566
C2 K1 C3 96.37(10) 3_556 3_566
C1 K1 C3 89.99(10) 4_566 3_566
C1 K1 C3 90.01(10) 2_545 3_566
C3 K1 C3 180.00(13) 1_545 3_566
C4 N1 H1A 109.5 . .
C4 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C4 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C2 O3 Cr1 126.1(2) . .
O6 C3 O5 125.9(4) . .
O6 C3 K1 48.4(2) . 1_565
O5 C3 K1 166.8(3) . 1_565
O6 C3 H3 117.1 . .
O5 C3 H3 117.1 . .
K1 C3 H3 70.1 1_565 .
O4 C2 O3 123.6(4) . .
O4 C2 K1 47.8(2) . .
O3 C2 K1 170.9(3) . .
O4 C2 H2 118.2 . .
O3 C2 H2 118.2 . .
K1 C2 H2 70.5 . .
C1 O2 K1 114.1(2) . 2
N1 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C2 O4 K1 112.3(2) . .
C3 O6 K1 112.0(3) . 1_565
C3 O5 Cr1 125.2(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O3 1.965(2) 3_666
Cr1 O3 1.965(2) .
Cr1 O1 1.969(2) 3_666
Cr1 O1 1.969(2) .
Cr1 O5 1.973(2) 3_666
Cr1 O5 1.973(2) .
O1 C1 1.267(4) .
C1 O2 1.232(4) .
C1 K1 3.399(4) 2
C1 H1 0.9300 .
K1 O4 2.677(3) .
K1 O4 2.677(3) 3_556
K1 O2 2.705(3) 4_566
K1 O2 2.705(3) 2_545
K1 O6 2.742(3) 3_566
K1 O6 2.742(3) 1_545
K1 C2 3.346(4) .
K1 C2 3.346(4) 3_556
K1 C1 3.399(4) 4_566
K1 C1 3.399(4) 2_545
K1 C3 3.399(4) 1_545
K1 C3 3.399(4) 3_566
N1 C4 1.476(5) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
O3 C2 1.269(4) .
C3 O6 1.229(4) .
C3 O5 1.261(4) .
C3 K1 3.399(4) 1_565
C3 H3 0.9300 .
C2 O4 1.232(4) .
C2 H2 0.9300 .
O2 K1 2.705(3) 2
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
O6 K1 2.742(3) 1_565
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 O6 0.89 1.94 2.833(4) 176.9 2_545
N1 H1B O2 0.89 1.95 2.821(4) 167.3 2_645
N1 H1C O3 0.89 2.58 3.283(4) 136.1 .
N1 H1C O4 0.89 1.92 2.795(4) 166.5 .
C3 H3 O3 0.93 2.53 3.016(5) 112.6 3_666
C2 H2 O1 0.93 2.51 2.998(5) 112.6 3_666
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
Cr1 O1 C1 O2 177.6(3) . .
Cr1 O3 C2 O4 175.4(3) . .
O1 C1 O2 K1 -177.4(3) . 2
O3 C2 O4 K1 176.1(3) . .
O5 C3 O6 K1 -164.7(3) . 1_565
O6 C3 O5 Cr1 -173.8(3) . .
K1 C3 O5 Cr1 126.4(11) 1_565 .
