#------------------------------------------------------------------------------ #$Date: 2020-10-06 14:19:17 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257997 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240557.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_7240557 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_page_last 19026 _journal_paper_doi 10.1039/D0RA03397A _journal_volume 10 _journal_year 2020 _chemical_formula_sum 'C1.17 H12.84 Mn N2 O6 P2.83' _chemical_formula_weight 293.60 _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 9.3938(6) _cell_length_b 13.3012(8) _cell_length_c 8.5716(6) _cell_measurement_reflns_used 3151 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 29.1630 _cell_measurement_theta_min 2.8060 _cell_volume 1071.01(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)' _diffrn_ambient_temperature 295(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.6249 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.904 _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 0.0303 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.904 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 6102 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.904 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.506 _diffrn_reflns_theta_min 2.827 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.657 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.96807 _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 1.821 _exptl_crystal_description prism _exptl_crystal_F_000 604 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.344 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 68 _refine_ls_number_reflns 1399 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.095 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0369 _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/[\s^2^(Fo^2^)+(0.0471P)^2^+1.8779P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0970 _refine_ls_wR_factor_ref 0.1063 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1111 _reflns_number_total 1399 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ra03397a2.cif _cod_data_source_block III _cod_depositor_comments 'Adding full bibliography for 7240557--7240559.cif.' _cod_database_code 7240557 _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 0.971 _oxdiff_exptl_absorpt_empirical_full_max 1.050 _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 rt.res created by SHELXL-2018/3 at 12:04:27 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 9.393833 13.301213 8.571560 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 51.36 8 24 11.32 4 4.68 L.S. 10 0 0 PLAN 20 BOND $H list 4 fmap 2 53 ACTA bond $H htab omit 4 2 1 omit 0 5 1 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 eadp p2 c2 exyz p2 c2 WGHT 0.046900 0.966800 FVAR 3.76743 MN1 5 0.500000 0.500000 0.500000 10.50000 0.02421 0.01488 = 0.02955 0.00079 -0.00084 -0.00061 P1 4 0.489750 0.750000 0.648211 10.50000 0.04530 0.01701 = 0.03448 0.00000 -0.00408 0.00000 AFIX 23 H1A 1 0.587670 0.750000 0.684129 10.50000 -1.20000 H1B 1 0.429515 0.750000 0.740127 10.50000 -1.20000 AFIX 0 P2 4 0.181612 0.515808 0.670367 10.91500 0.05403 0.02521 = 0.05452 0.00440 0.02517 0.00194 AFIX 23 H2A 1 0.121998 0.553198 0.598454 10.96000 -1.20000 H2B 1 0.231845 0.564449 0.734227 10.96000 -1.20000 AFIX 0 C2 6 0.181612 0.515808 0.670367 10.08500 0.05403 0.02521 = 0.05452 0.00440 0.02517 0.00194 O1 3 0.088082 0.456274 0.773131 11.00000 0.04920 0.02950 = 0.03904 -0.00342 0.01604 -0.00506 O2 3 0.287472 0.459723 0.578692 11.00000 0.03589 0.03293 = 0.05433 -0.00536 0.01380 -0.00667 O3 3 0.464858 0.655335 0.563773 11.00000 0.06521 0.01922 = 0.06522 -0.00990 -0.00397 0.00314 N2 2 0.177798 0.250000 0.763422 10.50000 0.02793 0.02686 = 0.04016 0.00000 0.00419 0.00000 AFIX 23 HB 1 0.131327 0.196068 0.797819 10.50000 -1.20000 HC 1 0.131327 0.303932 0.797820 10.50000 -1.20000 AFIX 0 N1 2 0.172583 0.250000 0.595150 10.50000 0.05629 0.02871 = 0.03951 0.00000 0.00387 0.00000 AFIX 7 HA 1 0.218763 0.198898 0.558596 11.00000 -1.20000 AFIX 0 C1 6 0.320881 0.250000 0.832828 10.50000 0.03227 0.04224 = 0.05429 0.00000 0.00178 0.00000 AFIX 133 HD 1 0.372054 0.191608 0.798360 10.50000 -1.50000 HE 1 0.313039 0.248938 0.944484 10.50000 -1.50000 HF 1 0.371000 0.309453 0.800970 10.50000 -1.50000 AFIX 0 HKLF 4 REM mhyd_mn_po2_30m_a.res in Pnma REM wR2 = 0.1063, GooF = S = 1.095, Restrained GooF = 1.095 for all data REM R1 = 0.0369 for 1111 Fo > 4sig(Fo) and 0.0497 for all 1399 data REM 68 parameters refined using 0 restraints END WGHT 0.0474 0.9735 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 0.344, deepest hole -0.662, 1-sigma level 0.085 Q1 1 0.0063 0.2500 0.8506 10.50000 0.05 0.34 Q2 1 0.2524 0.5904 0.7653 11.00000 0.05 0.32 Q3 1 0.4946 0.6570 0.4990 11.00000 0.05 0.30 Q4 1 0.3440 0.7500 0.7792 10.50000 0.05 0.30 Q5 1 0.4234 0.6567 0.5460 11.00000 0.05 0.29 Q6 1 0.5461 0.6538 0.5742 11.00000 0.05 0.25 Q7 1 0.2742 0.4555 0.6624 11.00000 0.05 0.24 Q8 1 0.3346 0.5569 0.7987 11.00000 0.05 0.24 Q9 1 0.1526 0.4932 0.5979 11.00000 0.05 0.24 Q10 1 0.5130 0.7500 0.8001 10.50000 0.05 0.24 Q11 1 0.0889 0.5786 0.5784 11.00000 0.05 0.24 Q12 1 0.1001 0.5594 0.4695 11.00000 0.05 0.23 Q13 1 0.2834 0.6598 0.7412 11.00000 0.05 0.23 Q14 1 0.6529 0.7500 0.7507 10.50000 0.05 0.23 Q15 1 0.1585 0.6055 0.6700 11.00000 0.05 0.22 Q16 1 0.0486 0.1388 0.7174 11.00000 0.05 0.22 Q17 1 0.4600 0.6464 0.6226 11.00000 0.05 0.22 Q18 1 0.1801 0.5433 0.6770 11.00000 0.05 0.22 Q19 1 0.0733 0.3802 0.7022 11.00000 0.05 0.21 Q20 1 0.3597 0.3341 0.8079 11.00000 0.05 0.21 ; _shelx_res_checksum 48410 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 0.02288(18) Uani 1 2 d S . P . . P1 P 0.48975(12) 0.750000 0.64821(12) 0.0323(3) Uani 1 2 d S T P . . H1A H 0.587670 0.750000 0.684129 0.039 Uiso 1 2 calc R U P . . H1B H 0.429515 0.750000 0.740127 0.039 Uiso 1 2 calc R U P . . P2 P 0.18161(11) 0.51581(6) 0.67037(12) 0.0446(3) Uani 0.915 1 d . . P . . H2A H 0.121998 0.553198 0.598454 0.054 Uiso 0.96 1 calc R U P . . H2B H 0.231845 0.564449 0.734227 0.054 Uiso 0.96 1 calc R U P . . C2 C 0.18161(11) 0.51581(6) 0.67037(12) 0.0446(3) Uani 0.085 1 d . . P . . O1 O 0.0881(2) 0.45627(14) 0.7731(2) 0.0392(5) Uani 1 1 d . . . . . O2 O 0.2875(2) 0.45972(15) 0.5787(3) 0.0410(5) Uani 1 1 d . . . . . O3 O 0.4649(3) 0.65533(15) 0.5638(3) 0.0499(6) Uani 1 1 d . . . . . N2 N 0.1778(3) 0.250000 0.7634(4) 0.0316(7) Uani 1 2 d S T P . . HB H 0.131327 0.196068 0.797819 0.038 Uiso 0.5 1 calc R U P . . HC H 0.131327 0.303932 0.797820 0.038 Uiso 0.5 1 calc R U P . . N1 N 0.1726(4) 0.250000 0.5951(4) 0.0415(9) Uani 1 2 d S T P . . HA H 0.218763 0.198898 0.558596 0.050 Uiso 1 1 d R U . . . C1 C 0.3209(5) 0.250000 0.8328(5) 0.0429(10) Uani 1 2 d S T P . . HD H 0.372054 0.191608 0.798360 0.064 Uiso 0.5 1 calc R U P . . HE H 0.313039 0.248938 0.944484 0.064 Uiso 0.5 2 calc R U P . . HF H 0.371000 0.309453 0.800970 0.064 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 0.0242(3) 0.0149(3) 0.0295(3) 0.00079(19) -0.0008(2) -0.00061(19) P1 0.0453(6) 0.0170(4) 0.0345(5) 0.000 -0.0041(4) 0.000 P2 0.0540(6) 0.0252(4) 0.0545(6) 0.0044(3) 0.0252(5) 0.0019(4) C2 0.0540(6) 0.0252(4) 0.0545(6) 0.0044(3) 0.0252(5) 0.0019(4) O1 0.0492(13) 0.0295(9) 0.0390(11) -0.0034(8) 0.0160(10) -0.0051(9) O2 0.0359(11) 0.0329(10) 0.0543(13) -0.0054(10) 0.0138(10) -0.0067(9) O3 0.0652(15) 0.0192(9) 0.0652(15) -0.0099(10) -0.0040(12) 0.0031(10) N2 0.0279(16) 0.0269(14) 0.0402(18) 0.000 0.0042(14) 0.000 N1 0.056(2) 0.0287(16) 0.0395(19) 0.000 0.0039(17) 0.000 C1 0.032(2) 0.042(2) 0.054(3) 0.000 0.002(2) 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 90.97(8) 5_666 5_666 ? O3 Mn1 O2 89.03(9) . 5_666 ? O3 Mn1 O2 89.04(9) 5_666 . ? O3 Mn1 O2 90.96(8) . . ? O2 Mn1 O2 180.0 5_666 . ? O3 Mn1 O1 85.01(8) 5_666 6_657 ? O3 Mn1 O1 94.98(8) . 6_657 ? O2 Mn1 O1 89.65(9) 5_666 6_657 ? O2 Mn1 O1 90.35(9) . 6_657 ? O3 Mn1 O1 94.99(8) 5_666 2_564 ? O3 Mn1 O1 85.02(8) . 2_564 ? O2 Mn1 O1 90.35(9) 5_666 2_564 ? O2 Mn1 O1 89.65(9) . 2_564 ? O1 Mn1 O1 180.0 6_657 2_564 ? O3 P1 O3 117.7(2) . 7_575 ? O3 P1 H1A 107.9 . . ? O3 P1 H1A 107.9 7_575 . ? O3 P1 H1B 107.9 . . ? O3 P1 H1B 107.9 7_575 . ? H1A P1 H1B 107.2 . . ? O2 P2 O1 116.72(12) . . ? O2 P2 H2A 108.1 . . ? O1 P2 H2A 108.1 . . ? O2 P2 H2B 108.1 . . ? O1 P2 H2B 108.1 . . ? H2A P2 H2B 107.3 . . ? P2 O1 Mn1 127.76(11) . 2_565 ? P2 O2 Mn1 131.42(12) . . ? P1 O3 Mn1 156.62(16) . . ? N1 N2 C1 115.8(3) . . ? N1 N2 HB 108.3 . . ? C1 N2 HB 108.3 . . ? N1 N2 HC 108.3 . . ? C1 N2 HC 108.3 . . ? HB N2 HC 107.4 . . ? N2 N1 HA 110.2 . . ? N2 N1 HA 110.2(7) . 7_565 ? HA N1 HA 103.6 . 7_565 ? N2 C1 HD 109.5 . . ? N2 C1 HE 109.5 . . ? HD C1 HE 109.5 . . ? N2 C1 HF 109.5 . . ? HD C1 HF 109.5 . . ? HE C1 HF 109.5 . . ? 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 2.163(2) 5_666 ? Mn1 O3 2.163(2) . ? Mn1 O2 2.174(2) 5_666 ? Mn1 O2 2.174(2) . ? Mn1 O1 2.1919(19) 6_657 ? Mn1 O1 2.1919(19) 2_564 ? P1 O3 1.471(2) . ? P1 O3 1.471(2) 7_575 ? P1 H1A 0.9700 . ? P1 H1B 0.9700 . ? P2 O2 1.471(2) . ? P2 O1 1.475(2) . ? P2 H2A 0.9700 . ? P2 H2B 0.9700 . ? N2 N1 1.443(5) . ? N2 C1 1.470(5) . ? N2 HB 0.8900 . ? N2 HC 0.8900 . ? N1 HA 0.8651 . ? N1 HA 0.87(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 2.08 2.871(2) 148.0 7_565 yes N2 HB O3 0.89 2.51 3.164(4) 130.6 8_656 yes N2 HC O1 0.89 2.08 2.871(2) 148.0 . yes N2 HC O3 0.89 2.51 3.164(4) 130.6 2_565 yes N1 HA O2 0.87 2.21 2.994(2) 150.1 7_565 yes