#------------------------------------------------------------------------------ #$Date: 2020-05-20 07:19:51 +0300 (Wed, 20 May 2020) $ #$Revision: 252202 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240558.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_7240558 loop_ _publ_author_name 'M\;aczka, Miros\/law' 'G\;agor, Anna' 'Pikul, Adam' 'Stefa\'nska, Dagmara' _publ_section_title ; Novel hypophosphite hybrid perovskites of [CH3NH2NH2][Mn(H2POO)3] and [CH3NH2NH2][Mn(H2POO)2.83(HCOO)0.17] exhibiting antiferromagnetic order and red photoluminescence ; _journal_issue 32 _journal_name_full 'RSC Advances' _journal_page_first 19020 _journal_paper_doi 10.1039/D0RA03397A _journal_volume 10 _journal_year 2020 _chemical_formula_sum 'C H13 Mn N2 O6 P3' _chemical_formula_weight 296.98 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-03-09 deposited with the CCDC. 2020-05-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.2009(6) _cell_length_b 13.2604(8) _cell_length_c 8.5408(6) _cell_measurement_reflns_used 5364 _cell_measurement_temperature 100.0(2) _cell_measurement_theta_max 29.2010 _cell_measurement_theta_min 2.8360 _cell_volume 1042.04(12) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.6249 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas' _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 0.0421 _diffrn_reflns_av_unetI/netI 0.0169 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 11095 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.673 _diffrn_reflns_theta_min 2.837 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.729 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.893 _exptl_crystal_description prism _exptl_crystal_F_000 604 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.435 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.080 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 68 _refine_ls_number_reflns 1037 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.183 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0284 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+1.7075P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.0829 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1014 _reflns_number_total 1037 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ra03397a2.cif _cod_data_source_block II _cod_database_code 7240558 _shelx_shelxl_version_number 2018/3 _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. ; _oxdiff_exptl_absorpt_empirical_full_min 0.847 _oxdiff_exptl_absorpt_empirical_full_max 1.368 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL mhyd_mn_po2_30m_a.res in Pnma 100K.res created by SHELXL-2018/3 at 13:43:56 on 02-Mar-2020 REM Old TITL MHyd_Mn_PO2_30m in Pnma REM SHELXT solution in Pnma REM R1 0.121, Rweak 0.143, Alpha 0.033, Orientation as input CELL 0.71073 9.2009 13.2604 8.5408 90 90 90 ZERR 4 0.000586 0.00076 0.000608 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC H N O P Mn C UNIT 52 8 24 12 4 4 L.S. 10 0 0 PLAN 20 BOND $H list 4 fmap 2 53 shel 10 0.82 omit 0 4 0 ACTA bond $H htab EQIV $6 x, -y+1/2, z HTAB N2 O1_$6 EQIV $7 -x+1/2, y-1/2, z+1/2 HTAB N2 O3_$7 HTAB N2 O1 EQIV $1 -x+1/2, -y+1, z+1/2 HTAB N2 O3_$1 HTAB N1 O2_$6 WGHT 0.036900 1.707500 EXTI 0.002275 FVAR 0.35192 MN1 5 0.500000 0.500000 0.500000 10.50000 0.00667 0.00479 = 0.02322 -0.00010 -0.00041 -0.00014 P1 4 0.489997 0.750000 0.650497 10.50000 0.01147 0.00731 = 0.02533 0.00000 -0.00119 0.00000 AFIX 23 H1A 1 0.591560 0.750001 0.680953 10.50000 -1.20000 H1B 1 0.432834 0.750000 0.745925 10.50000 -1.20000 AFIX 0 P2 4 0.173766 0.516450 0.664897 11.00000 0.01515 0.00800 = 0.02901 0.00075 0.00557 0.00020 AFIX 23 H2A 1 0.113083 0.557074 0.596729 11.00000 -1.20000 H2B 1 0.228395 0.562375 0.730860 11.00000 -1.20000 AFIX 0 O1 3 0.076192 0.454384 0.768161 11.00000 0.01330 0.01103 = 0.02651 -0.00085 0.00411 -0.00166 O2 3 0.279331 0.459284 0.565019 11.00000 0.01073 0.01269 = 0.02867 -0.00221 0.00343 -0.00360 O3 3 0.459987 0.654466 0.565409 11.00000 0.02104 0.00794 = 0.03740 -0.00312 -0.00287 0.00171 N2 2 0.170490 0.250000 0.762288 10.50000 0.00811 0.00892 = 0.02853 0.00000 0.00135 0.00000 AFIX 23 HB 1 0.123156 0.195890 0.796942 10.50000 -1.20000 HC 1 0.123156 0.304110 0.796942 10.50000 -1.20000 AFIX 0 N1 2 0.165082 0.250000 0.593361 10.50000 0.01888 0.00893 = 0.02650 0.00000 0.00187 0.00000 AFIX 7 HA 1 0.212481 0.199570 0.555645 11.00000 -1.20000 AFIX 0 C1 6 0.318744 0.250000 0.831987 10.50000 0.00919 0.01447 = 0.03239 0.00000 -0.00138 0.00000 AFIX 133 HD 1 0.370645 0.191246 0.797540 10.50000 -1.50000 HE 1 0.311276 0.249292 0.944095 10.50000 -1.50000 HF 1 0.369938 0.309462 0.799284 10.50000 -1.50000 AFIX 0 HKLF 4 REM mhyd_mn_po2_30m_a.res in Pnma REM wR2 = 0.0829, GooF = S = 1.183, Restrained GooF = 1.183 for all data REM R1 = 0.0284 for 1014 Fo > 4sig(Fo) and 0.0290 for all 1037 data REM 69 parameters refined using 0 restraints END WGHT 0.0365 1.7088 REM Instructions for potential hydrogen bonds HTAB N2 O1_$6 HTAB N2 O3_$7 HTAB N2 O1 HTAB N2 O3_$1 HTAB N1 O2_$6 REM Highest difference peak 0.435, deepest hole -0.466, 1-sigma level 0.080 Q1 1 0.4057 0.7500 0.8204 10.50000 0.05 0.43 Q2 1 0.6520 0.7500 0.7221 10.50000 0.05 0.43 Q3 1 0.2582 0.5947 0.7641 11.00000 0.05 0.41 Q4 1 0.0793 0.5799 0.5435 11.00000 0.05 0.40 Q5 1 0.4826 0.6996 0.5716 11.00000 0.05 0.32 Q6 1 0.1144 0.4788 0.7260 11.00000 0.05 0.29 Q7 1 0.1405 0.4606 0.7418 11.00000 0.05 0.29 Q8 1 0.2397 0.2500 0.7972 10.50000 0.05 0.26 Q9 1 0.0887 0.4354 0.8037 11.00000 0.05 0.25 Q10 1 0.2769 0.4829 0.5067 11.00000 0.05 0.23 Q11 1 0.5059 0.4521 0.4233 11.00000 0.05 0.22 Q12 1 0.0663 0.4165 0.7184 11.00000 0.05 0.22 Q13 1 0.4596 0.6581 0.4996 11.00000 0.05 0.22 Q14 1 0.2398 0.5048 0.5647 11.00000 0.05 0.22 Q15 1 0.2064 0.4787 0.5854 11.00000 0.05 0.21 Q16 1 0.5059 0.4525 0.5815 11.00000 0.05 0.21 Q17 1 0.2458 0.4210 0.5429 11.00000 0.05 0.18 Q18 1 0.0739 0.2500 0.5433 10.50000 0.05 0.18 Q19 1 0.0209 0.4766 0.7847 11.00000 0.05 0.18 Q20 1 0.5859 0.7500 0.8332 10.50000 0.05 0.16 ; _shelx_res_checksum 68266 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, 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 _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.500000 0.500000 0.500000 0.0116(2) Uani 1 2 d S . P . . P1 P 0.49000(9) 0.750000 0.65050(11) 0.0147(3) Uani 1 2 d S T P . . H1A H 0.591560 0.750001 0.680953 0.018 Uiso 1 2 calc R U P . . H1B H 0.432834 0.750000 0.745925 0.018 Uiso 1 2 calc R U P . . P2 P 0.17377(7) 0.51645(5) 0.66490(8) 0.0174(2) Uani 1 1 d . . . . . H2A H 0.113083 0.557074 0.596729 0.021 Uiso 1 1 calc R U . . . H2B H 0.228395 0.562375 0.730860 0.021 Uiso 1 1 calc R U . . . O1 O 0.07619(17) 0.45438(12) 0.7682(2) 0.0169(4) Uani 1 1 d . . . . . O2 O 0.27933(17) 0.45928(12) 0.5650(2) 0.0174(4) Uani 1 1 d . . . . . O3 O 0.4600(2) 0.65447(13) 0.5654(2) 0.0221(4) Uani 1 1 d . . . . . N2 N 0.1705(3) 0.250000 0.7623(4) 0.0152(6) Uani 1 2 d S T P . . HB H 0.123156 0.195890 0.796942 0.018 Uiso 0.5 1 calc R U P . . HC H 0.123156 0.304110 0.796942 0.018 Uiso 0.5 1 calc R U P . . N1 N 0.1651(3) 0.250000 0.5934(4) 0.0181(6) Uani 1 2 d S T P . . HA H 0.212481 0.199570 0.555645 0.022 Uiso 1 1 d R U . . . C1 C 0.3187(4) 0.250000 0.8320(5) 0.0187(8) Uani 1 2 d S T P . . HD H 0.370645 0.191246 0.797540 0.028 Uiso 0.5 1 calc R U P . . HE H 0.311276 0.249292 0.944095 0.028 Uiso 0.5 2 calc R U P . . HF H 0.369938 0.309462 0.799284 0.028 Uiso 0.5 1 calc R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0067(3) 0.0048(3) 0.0232(4) -0.00010(18) -0.00041(18) -0.00014(16) P1 0.0115(4) 0.0073(4) 0.0253(5) 0.000 -0.0012(3) 0.000 P2 0.0152(4) 0.0080(3) 0.0290(4) 0.0007(2) 0.0056(3) 0.0002(2) O1 0.0133(8) 0.0110(8) 0.0265(10) -0.0008(7) 0.0041(7) -0.0017(6) O2 0.0107(8) 0.0127(8) 0.0287(9) -0.0022(7) 0.0034(7) -0.0036(7) O3 0.0210(9) 0.0079(8) 0.0374(11) -0.0031(7) -0.0029(8) 0.0017(7) N2 0.0081(13) 0.0089(13) 0.0285(16) 0.000 0.0014(11) 0.000 N1 0.0189(15) 0.0089(13) 0.0265(16) 0.000 0.0019(13) 0.000 C1 0.0092(16) 0.0145(17) 0.032(2) 0.000 -0.0014(14) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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 _geom_angle_publ_flag O3 Mn1 O3 180.0 5_666 . ? O3 Mn1 O2 90.59(7) 5_666 5_666 ? O3 Mn1 O2 89.41(7) . 5_666 ? O3 Mn1 O2 89.41(7) 5_666 . ? O3 Mn1 O2 90.59(7) . . ? O2 Mn1 O2 180.0 5_666 . ? O3 Mn1 O1 85.24(7) 5_666 6_657 ? O3 Mn1 O1 94.76(7) . 6_657 ? O2 Mn1 O1 90.03(7) 5_666 6_657 ? O2 Mn1 O1 89.97(7) . 6_657 ? O3 Mn1 O1 94.76(7) 5_666 2_564 ? O3 Mn1 O1 85.24(7) . 2_564 ? O2 Mn1 O1 89.97(7) 5_666 2_564 ? O2 Mn1 O1 90.03(7) . 2_564 ? O1 Mn1 O1 180.0 6_657 2_564 ? O3 P1 O3 116.93(16) . 7_575 ? O3 P1 H1A 108.1 . . ? O3 P1 H1A 108.1 7_575 . ? O3 P1 H1B 108.1 . . ? O3 P1 H1B 108.1 7_575 . ? O2 P2 O1 116.36(10) . . ? O2 P2 H2A 108.2 . . ? O1 P2 H2A 108.2 . . ? O2 P2 H2B 108.2 . . ? O1 P2 H2B 108.2 . . ? P2 O1 Mn1 124.84(10) . 2_565 ? P2 O2 Mn1 128.71(10) . . ? P1 O3 Mn1 154.85(12) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3 2.1548(17) 5_666 ? Mn1 O3 2.1548(17) . ? Mn1 O2 2.1731(16) 5_666 ? Mn1 O2 2.1731(16) . ? Mn1 O1 2.1859(17) 6_657 ? Mn1 O1 2.1859(17) 2_564 ? P1 O3 1.4863(18) . ? P1 O3 1.4864(18) 7_575 ? P1 H1A 0.9700 . ? P1 H1B 0.9700 . ? P2 O2 1.4986(18) . ? P2 O1 1.5037(17) . ? P2 H2A 0.9700 . ? P2 H2B 0.9700 . ? N2 N1 1.444(4) . ? N2 C1 1.488(4) . ? N2 HB 0.8900 . ? N2 HC 0.8900 . ? N1 HA 0.8609 . ? N1 HA 0.86(3) 7_565 ? C1 HD 0.9600 . ? C1 HE 0.9600 . ? C1 HF 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 _geom_hbond_publ_flag N2 HB O1 0.89 2.05 2.8461(18) 147.7 7_565 yes N2 HB O3 0.89 2.48 3.122(3) 129.6 8_656 yes N2 HC O1 0.89 2.05 2.8461(18) 147.7 . yes N2 HC O3 0.89 2.48 3.122(3) 129.6 2_565 yes N1 HA O2 0.86 2.20 2.977(2) 150.9 7_565 yes