#------------------------------------------------------------------------------
#$Date: 2025-07-06 17:13:19 +0200 (Sun 06 de Jul de 2025) $
#$Revision: 300733 $
#$URL: svn://www.crystallography.net/cod/cif/7/25/02/7250256.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_7250256
loop_
_publ_author_name
'Matsuda, Yumi'
'Asai, Rentaro'
'Moriguchi, Jumpei'
'Akutagawa, Tomoyuki'
'Masuya-Suzuki, Atsuko'
'Tsunashima, Ryo'
_publ_section_title
;
 Synthesis, crystallographic study and solid-state properties of
 metal-free perovskites with P-atom containing A-site cations
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              2824
_journal_page_last               2829
_journal_paper_doi               10.1039/D5CE00177C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         '3(I), C6 H14 N3 P, H4 N'
_chemical_formula_sum            'C6 H18 I3 N4 P'
_chemical_formula_weight         557.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-01-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-17 deposited with the CCDC.	2025-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1395(5)
_cell_length_b                   14.4681(5)
_cell_length_c                   14.2255(4)
_cell_measurement_reflns_used    6324
_cell_measurement_temperature    253
_cell_measurement_theta_max      30.6960
_cell_measurement_theta_min      2.4790
_cell_volume                     2910.13(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      253
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  64.00   0.25    0.17    --   -5.68  71.00  50.00  364
  2  ω    -16.00  39.00   0.25    0.17    --    6.15 -99.00-150.00  220
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0023918000
_diffrn_orient_matrix_UB_12      0.0314373000
_diffrn_orient_matrix_UB_13      -0.0381592000
_diffrn_orient_matrix_UB_21      -0.0466342000
_diffrn_orient_matrix_UB_22      0.0152422000
_diffrn_orient_matrix_UB_23      0.0099217000
_diffrn_orient_matrix_UB_31      0.0182697000
_diffrn_orient_matrix_UB_32      0.0344279000
_diffrn_orient_matrix_UB_33      0.0305166000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6432
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.471
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.531
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.547
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.00102(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1547
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0211
_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/[σ²(Fo²)+(0.0312P)²+4.1922P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1493
_reflns_number_total             1547
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00177c2.cif
_cod_data_source_block           p-i_253k
_cod_depositor_comments
'Adding full bibliography for 7250254--7250270.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7250256
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C6H18N3IP
_chemical_oxdiff_usercomment     'solid solution 7-3'
_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.
;
_shelx_estimated_absorpt_t_max   0.403
_shelx_estimated_absorpt_t_min   0.237
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H,H,H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H,H) groups
2. Restrained distances
 C1-H1A = C1-H1B
 1.09 with sigma of 0.02
 N1-H1C = N1-H1D = N1-H1E
 1.06 with sigma of 0.02
 H1A-H1B
 1.78 with sigma of 0.04
 H1C-H1D = H1C-H1E = H1D-H1E
 1.75 with sigma of 0.04
3. Others
 Fixed Sof: P1(0.5) H4A(0.5) H4B(0.5) C1(0.5) N2(0.5) H1A(0.5) H1B(0.5)
4.a Ternary CH refined with riding coordinates:
 N3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.874
_oxdiff_exptl_absorpt_empirical_full_min 0.593
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'
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
I001 I 0.500000 0.46065(2) 0.72612(2) 0.02498(11) Uani 1 2 d S T P . .
I002 I 0.500000 0.27105(2) 0.47967(2) 0.02679(11) Uani 1 2 d S T P . .
I003 I 0.750000 0.25494(2) 0.750000 0.03017(11) Uani 1 2 d S T P . .
P1 P 0.1565(2) 0.5684(3) 0.5709(3) 0.0220(6) Uani 0.5 1 d . . P A 1
N1 N 0.500000 0.2071(3) 0.7243(3) 0.0320(9) Uani 1 2 d DS T P . .
N3 N 0.30484(18) 0.44008(17) 0.55984(16) 0.0218(5) Uani 1 1 d . . . . .
H3 H 0.347003 0.401428 0.599099 0.026 Uiso 1 1 calc R U . . .
C3 C 0.2442(2) 0.3753(2) 0.5008(2) 0.0286(7) Uani 1 1 d . . . . .
C4 C 0.3659(3) 0.500000 0.500000 0.0264(9) Uani 1 2 d S T P . .
H4A H 0.406494 0.538459 0.539834 0.032 Uiso 0.5 1 calc R U P . .
H4B H 0.406491 0.461540 0.460164 0.032 Uiso 0.5 1 calc R U P . .
C2 C 0.2446(2) 0.4985(2) 0.6259(2) 0.0287(7) Uani 1 1 d . . . . .
C1 C 0.1129(4) 0.5165(5) 0.5162(5) 0.0234(16) Uani 0.5 1 d D . P . .
N2 N 0.1905(6) 0.5669(10) 0.5675(9) 0.025(2) Uani 0.5 1 d . . P A -1
H3A H 0.205(3) 0.341(3) 0.546(3) 0.029 Uiso 1 1 d . U . . .
H3B H 0.290(3) 0.335(3) 0.460(3) 0.029 Uiso 1 1 d . U . . .
H2A H 0.209(3) 0.454(3) 0.667(3) 0.029 Uiso 1 1 d . U . . .
H2B H 0.291(3) 0.535(3) 0.665(3) 0.029 Uiso 1 1 d . U . . .
H1A H 0.068(4) 0.480(4) 0.566(4) 0.022(16) Uiso 0.5 1 d D . P B -1
H1B H 0.071(5) 0.571(4) 0.482(5) 0.04(2) Uiso 0.5 1 d D . P C -1
H1C H 0.500000 0.1361(16) 0.742(4) 0.048 Uiso 1 2 d DS U P . .
H1D H 0.500000 0.220(4) 0.6509(15) 0.048 Uiso 1 2 d DS U P . .
H1E H 0.565(2) 0.235(3) 0.748(3) 0.048 Uiso 1 1 d D U . . .
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'
I I -0.4742 1.8119 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 20 0 0.1295
8 4 18 0.1492
5 -12 15 0.1474
-8 -9 -16 0.0668
-3 17 -11 0.1195
-6 12 15 0.0835
-19 1 7 0.0658
3 -13 -15 0.0855
19 0 -7 0.1073
-16 -3 11 0.0825
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
C3 P1 C1 98.7(3) 4_566 4_566 ?
C2 P1 C3 91.4(2) . 4_566 ?
C2 P1 C1 98.6(3) . 4_566 ?
C1 P1 C3 105.1(4) . 4_566 ?
C1 P1 C2 106.1(5) . . ?
C1 P1 C1 10.23(19) . 4_566 ?
H1C N1 H1D 114(3) . . ?
H1C N1 H1E 107(2) . . ?
H1D N1 H1E 104(2) . . ?
C3 N3 H3 107.6 . . ?
C3 N3 C2 111.5(2) . . ?
C4 N3 H3 107.6 . . ?
C4 N3 C3 111.7(2) . . ?
C4 N3 C2 110.7(2) . . ?
C2 N3 H3 107.6 . . ?
P1 C3 H3A 102(2) 4_566 . ?
P1 C3 H3B 112(2) 4_566 . ?
N3 C3 P1 114.9(3) . 4_566 ?
N3 C3 H3A 106(2) . . ?
N3 C3 H3B 107(2) . . ?
H3A C3 H3B 115(3) . . ?
N3 C4 N3 109.2(3) 4_566 . ?
N3 C4 H4A 109.8 . . ?
N3 C4 H4A 109.8 4_566 . ?
N3 C4 H4B 109.8 4_566 . ?
N3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
P1 C2 H2A 106(2) . . ?
P1 C2 H2B 114(2) . . ?
N3 C2 P1 115.7(2) . . ?
N3 C2 H2A 106(2) . . ?
N3 C2 H2B 106(2) . . ?
N2 C2 P1 13.7(4) . . ?
N2 C2 N3 108.0(5) . . ?
N2 C2 H2A 119(2) . . ?
N2 C2 H2B 107(2) . . ?
H2A C2 H2B 110(3) . . ?
P1 C1 P1 130.9(5) . 4_566 ?
P1 C1 N2 17.1(5) . . ?
P1 C1 H1A 108(4) 4_566 . ?
P1 C1 H1A 100(4) . . ?
P1 C1 H1B 111(5) 4_566 . ?
P1 C1 H1B 96(4) . . ?
C1 C1 P1 19.5(2) 4_566 4_566 ?
C1 C1 P1 150.3(3) 4_566 . ?
C1 C1 N2 133.2(5) 4_566 . ?
C1 C1 H1A 96(4) 4_566 . ?
C1 C1 H1B 102(5) 4_566 . ?
N2 C1 P1 113.8(5) . 4_566 ?
N2 C1 H1A 111(4) . . ?
N2 C1 H1B 105(4) . . ?
H1A C1 H1B 109(3) . . ?
C2 N2 C1 108.7(9) . . ?
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
P1 C3 1.801(5) 4_566 ?
P1 C2 1.785(5) . ?
P1 C1 1.245(7) . ?
P1 C1 1.851(6) 4_566 ?
N1 H1C 1.058(18) . ?
N1 H1D 1.059(18) . ?
N1 H1E 1.066(18) . ?
N3 H3 0.9900 . ?
N3 C3 1.523(4) . ?
N3 C4 1.490(4) . ?
N3 C2 1.525(4) . ?
C3 H3A 0.98(4) . ?
C3 H3B 1.05(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C2 N2 1.501(13) . ?
C2 H2A 1.00(4) . ?
C2 H2B 1.01(4) . ?
C1 C1 0.663(10) 4_566 ?
C1 N2 1.506(12) . ?
C1 H1A 1.09(2) . ?
C1 H1B 1.09(2) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C2 N2 C1 -53(2) . . . . ?
P1 C1 N2 C2 -65.0(9) 4_566 . . . ?
P1 C1 N2 C2 112(2) . . . . ?
N3 C2 N2 C1 73.2(7) . . . . ?
C3 P1 C2 N3 -56.8(3) 4_566 . . . ?
C3 P1 C2 N2 2(3) 4_566 . . . ?
C3 P1 C1 P1 49.1(9) 4_566 . . 4_566 ?
C3 P1 C1 C1 52(4) 4_566 . . 4_566 ?
C3 P1 C1 N2 46(2) 4_566 . . . ?
C3 N3 C4 N3 62.58(19) . . . 4_566 ?
C3 N3 C2 P1 -57.9(3) . . . . ?
C3 N3 C2 N2 -70.2(5) . . . . ?
C4 N3 C3 P1 -66.0(3) . . . 4_566 ?
C4 N3 C2 P1 67.0(3) . . . . ?
C4 N3 C2 N2 54.8(5) . . . . ?
C2 P1 C1 P1 -46.9(9) . . . 4_566 ?
C2 P1 C1 C1 -44(4) . . . 4_566 ?
C2 P1 C1 N2 -50(2) . . . . ?
C2 N3 C3 P1 58.4(3) . . . 4_566 ?
C2 N3 C4 N3 -62.32(18) . . . 4_566 ?
C1 P1 C2 N3 42.2(4) 4_566 . . . ?
C1 P1 C2 N3 49.3(5) . . . . ?
C1 P1 C2 N2 108(3) . . . . ?
C1 P1 C2 N2 100(3) 4_566 . . . ?
C1 P1 C1 P1 -3(3) 4_566 . . 4_566 ?
C1 P1 C1 N2 -6(5) 4_566 . . . ?
C1 C1 N2 C2 -63(3) 4_566 . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.3767 20.2446 -0.4157 0.6580 0.1936 0.7277
8.4878 3.5689 17.7961 -0.5466 -0.1649 0.8210
5.3223 -12.1376 15.1920 -0.9486 -0.2825 0.1430
-8.3252 -9.0398 -15.9013 0.3027 0.0927 -0.9486
-2.9185 16.6854 -11.1442 0.9428 0.2799 0.1810
-6.3315 12.2804 14.6732 -0.1890 0.6280 0.7549
-18.8139 0.5231 6.6562 -0.2825 0.9514 -0.1226
3.4212 -13.3092 -14.7835 0.1539 -0.5091 -0.8468
18.8555 -0.4017 -6.5450 0.2822 -0.9504 0.1309
-16.3768 -3.4134 10.9827 -0.5656 0.8207 -0.0816
