#------------------------------------------------------------------------------
#$Date: 2019-03-30 04:26:39 +0200 (Sat, 30 Mar 2019) $
#$Revision: 214424 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/25/7232550.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_7232550
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 N2 Na O12'
_chemical_formula_weight         409.23
_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
;
2018-04-13 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.989(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9504(9)
_cell_length_b                   8.7582(10)
_cell_length_c                   11.8530(14)
_cell_measurement_reflns_used    5450
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      25.995
_cell_measurement_theta_min      3.110
_cell_volume                     825.22(16)
_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 0.992
_diffrn_measured_fraction_theta_max 0.993
_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  0.0509
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5450
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         3.110
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'slightly purple'
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0334
_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)+(0.0272P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1066
_reflns_number_total             1614
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cp01043b2.cif
_cod_data_source_block           100K
_cod_database_code               7232550
_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 0.01175(16) Uani 1 2 d S . P
O1 O 0.6282(2) 0.47331(19) 0.35992(15) 0.0138(4) Uani 1 1 d . . .
N1 N 0.9944(3) 0.4447(2) 0.2380(2) 0.0234(6) Uani 1 1 d . . .
H1A H 0.8876 0.4328 0.2162 0.035 Uiso 1 1 calc R U .
H1B H 1.0152 0.3879 0.2989 0.035 Uiso 1 1 calc R U .
H1C H 1.0615 0.4157 0.1826 0.035 Uiso 1 1 calc R U .
C1 C 0.5696(3) 0.4894(3) 0.2603(2) 0.0154(6) Uani 1 1 d . . .
H1 H 0.4594 0.5234 0.2514 0.019 Uiso 1 1 calc R U .
Na1 Na 1.0000 0.0000 0.5000 0.0167(3) Uani 1 2 d S . P
C3 C 0.7036(3) 0.2260(3) 0.5281(2) 0.0188(7) Uani 1 1 d . . .
H3 H 0.7710 0.2680 0.4728 0.023 Uiso 1 1 calc R U .
O3 O 0.2974(2) 0.4106(2) 0.42757(15) 0.0141(4) Uani 1 1 d . . .
C2 C 0.2178(3) 0.2951(3) 0.4639(2) 0.0162(6) Uani 1 1 d . . .
H2 H 0.2630 0.2438 0.5261 0.019 Uiso 1 1 calc R U .
O2 O 0.6500(2) 0.46258(19) 0.17454(15) 0.0189(5) Uani 1 1 d . . .
O4 O 0.0855(2) 0.2467(2) 0.42283(17) 0.0196(5) Uani 1 1 d . . .
C4 C 1.0257(4) 0.6058(3) 0.2649(3) 0.0311(8) Uani 1 1 d . . .
H4A H 0.9976 0.6676 0.2005 0.047 Uiso 1 1 calc R U .
H4B H 1.1423 0.6196 0.2847 0.047 Uiso 1 1 calc R U .
H4C H 0.9575 0.6356 0.3273 0.047 Uiso 1 1 calc R U .
O6 O 0.7475(2) 0.1047(2) 0.57049(16) 0.0212(5) Uani 1 1 d . . .
O5 O 0.5722(2) 0.29766(19) 0.55512(15) 0.0138(4) 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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
O5 Cr1 O5 180.0 3_666 .
O5 Cr1 O3 88.96(7) 3_666 .
O5 Cr1 O3 91.04(7) . .
O5 Cr1 O3 91.04(7) 3_666 3_666
O5 Cr1 O3 88.96(7) . 3_666
O3 Cr1 O3 180.0 . 3_666
O5 Cr1 O1 88.81(7) 3_666 .
O5 Cr1 O1 91.19(7) . .
O3 Cr1 O1 90.94(7) . .
O3 Cr1 O1 89.06(7) 3_666 .
O5 Cr1 O1 91.19(7) 3_666 3_666
O5 Cr1 O1 88.81(7) . 3_666
O3 Cr1 O1 89.06(7) . 3_666
O3 Cr1 O1 90.94(7) 3_666 3_666
O1 Cr1 O1 180.0 . 3_666
C1 O1 Cr1 125.60(17) . .
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 . .
O2 C1 O1 124.0(3) . .
O2 C1 Na1 43.73(13) . 2_655
O1 C1 Na1 167.69(19) . 2_655
O2 C1 H1 118.0 . .
O1 C1 H1 118.0 . .
Na1 C1 H1 74.3 2_655 .
O6 Na1 O6 180.0 3_756 .
O6 Na1 O2 86.86(7) 3_756 4_666
O6 Na1 O2 93.14(7) . 4_666
O6 Na1 O2 93.14(7) 3_756 2_645
O6 Na1 O2 86.86(7) . 2_645
O2 Na1 O2 180.0 4_666 2_645
O6 Na1 O4 91.86(6) 3_756 3_656
O6 Na1 O4 88.14(6) . 3_656
O2 Na1 O4 86.28(6) 4_666 3_656
O2 Na1 O4 93.72(6) 2_645 3_656
O6 Na1 O4 88.14(6) 3_756 1_655
O6 Na1 O4 91.86(6) . 1_655
O2 Na1 O4 93.72(6) 4_666 1_655
O2 Na1 O4 86.28(6) 2_645 1_655
O4 Na1 O4 180.0 3_656 1_655
O6 Na1 C3 159.11(7) 3_756 .
O6 Na1 C3 20.89(7) . .
O2 Na1 C3 100.83(7) 4_666 .
O2 Na1 C3 79.17(7) 2_645 .
O4 Na1 C3 107.88(7) 3_656 .
O4 Na1 C3 72.12(7) 1_655 .
O6 Na1 C3 20.89(7) 3_756 3_756
O6 Na1 C3 159.11(7) . 3_756
O2 Na1 C3 79.17(7) 4_666 3_756
O2 Na1 C3 100.83(7) 2_645 3_756
O4 Na1 C3 72.12(7) 3_656 3_756
O4 Na1 C3 107.88(7) 1_655 3_756
C3 Na1 C3 180.0 . 3_756
O6 Na1 C1 77.14(7) 3_756 2_645
O6 Na1 C1 102.86(7) . 2_645
O2 Na1 C1 159.15(6) 4_666 2_645
O2 Na1 C1 20.85(6) 2_645 2_645
O4 Na1 C1 107.28(7) 3_656 2_645
O4 Na1 C1 72.72(7) 1_655 2_645
C3 Na1 C1 90.18(7) . 2_645
C3 Na1 C1 89.82(7) 3_756 2_645
O6 Na1 C1 102.86(7) 3_756 4_666
O6 Na1 C1 77.14(7) . 4_666
O2 Na1 C1 20.85(6) 4_666 4_666
O2 Na1 C1 159.15(6) 2_645 4_666
O4 Na1 C1 72.72(7) 3_656 4_666
O4 Na1 C1 107.28(7) 1_655 4_666
C3 Na1 C1 89.82(7) . 4_666
C3 Na1 C1 90.18(7) 3_756 4_666
C1 Na1 C1 180.000(17) 2_645 4_666
O6 C3 O5 123.9(3) . .
O6 C3 Na1 43.78(13) . .
O5 C3 Na1 167.7(2) . .
O6 C3 H3 118.0 . .
O5 C3 H3 118.0 . .
Na1 C3 H3 74.3 . .
C2 O3 Cr1 125.10(18) . .
O4 C2 O3 124.6(3) . .
O4 C2 H2 117.7 . .
O3 C2 H2 117.7 . .
C1 O2 Na1 115.42(17) . 2_655
C2 O4 Na1 113.48(18) . 1_455
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 . .
C3 O6 Na1 115.34(18) . .
C3 O5 Cr1 126.85(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O5 1.9708(17) 3_666
Cr1 O5 1.9708(17) .
Cr1 O3 1.9743(17) .
Cr1 O3 1.9743(17) 3_666
Cr1 O1 1.9770(17) .
Cr1 O1 1.9770(17) 3_666
O1 C1 1.270(3) .
N1 C4 1.467(3) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
C1 O2 1.232(3) .
C1 Na1 3.126(3) 2_655
C1 H1 0.9300 .
Na1 O6 2.3725(18) 3_756
Na1 O6 2.3725(18) .
Na1 O2 2.3925(18) 4_666
Na1 O2 2.3925(18) 2_645
Na1 O4 2.4469(18) 3_656
Na1 O4 2.4469(18) 1_655
Na1 C3 3.099(3) .
Na1 C3 3.099(3) 3_756
Na1 C1 3.126(3) 2_645
Na1 C1 3.126(3) 4_666
C3 O6 1.223(3) .
C3 O5 1.265(3) .
C3 H3 0.9300 .
O3 C2 1.272(3) .
C2 O4 1.227(3) .
C2 H2 0.9300 .
O2 Na1 2.3925(18) 2_655
O4 Na1 2.4469(18) 1_455
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
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 1.96 2.832(3) 165.4 .
N1 H1B O4 0.89 1.99 2.877(3) 172.2 1_655
N1 H1C O6 0.89 2.01 2.884(3) 165.7 4_665
N1 H1C O5 0.89 2.41 3.104(3) 135.5 4_665
C3 H3 O1 0.93 2.50 2.998(3) 113.6 .
C3 H3 O4 0.93 2.59 3.307(3) 134.7 1_655
C2 H2 O5 0.93 2.52 3.001(3) 112.4 .
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_4
Cr1 O1 C1 O2 -175.23(19) .
Cr1 O1 C1 Na1 -171.4(7) 2_655
Cr1 O3 C2 O4 174.73(19) .
O1 C1 O2 Na1 178.8(2) 2_655
O3 C2 O4 Na1 170.8(2) 1_455
O5 C3 O6 Na1 179.7(2) .
O6 C3 O5 Cr1 175.2(2) .
Na1 C3 O5 Cr1 176.1(8) .
