#------------------------------------------------------------------------------
#$Date: 2024-07-05 03:16:25 +0200 (Fri 05 de Jul de 2024) $
#$Revision: 292747 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/89/7248981.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_7248981
loop_
_publ_author_name
'Guerriero, Antonella'
'Ienco, Andrea'
'Hicks, Thomas'
'Cilibrizzi, Agostino'
_publ_section_title
;
 Beyond transition block metals: exploring the reactivity of phosphine PTA
 and its oxide [PTA(O)] towards gallium(iii)
;
_journal_issue                   29
_journal_name_full               'RSC Advances'
_journal_page_first              21139
_journal_page_last               21150
_journal_paper_doi               10.1039/D4RA02877E
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C6 H13 N3 O P, I'
_chemical_formula_sum            'C6 H13 I N3 O P'
_chemical_formula_weight         301.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-03-19 deposited with the CCDC.	2024-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8486(3)
_cell_length_b                   9.6385(3)
_cell_length_c                   12.7790(4)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.17
_cell_measurement_theta_min      2.65
_cell_volume                     966.31(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53622
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.216
_diffrn_reflns_theta_min         2.596
_exptl_absorpt_coefficient_mu    3.439
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         3699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0159
_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)+(0.0096P)²+0.8259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0319
_refine_ls_wR_factor_ref         0.0334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3341
_reflns_number_total             3699
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra02877e2.cif
_cod_data_source_block           shelx_CCDC2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7248981
_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.
;
_shelx_estimated_absorpt_t_min   0.820
_shelx_estimated_absorpt_t_max   0.875
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
P1 P 0.23468(4) 0.22533(4) 0.74681(3) 0.00951(6) Uani 1 1 d . . . . .
O1 O 0.18370(12) 0.09944(11) 0.68543(8) 0.01345(18) Uani 1 1 d . . . . .
I1 I 0.19829(2) 0.67476(2) 0.49004(2) 0.01144(2) Uani 1 1 d . . . . .
N1 N 0.11389(14) 0.46172(12) 0.83445(8) 0.00999(19) Uani 1 1 d . . . . .
H1 H 0.0237(18) 0.5159(11) 0.8467(3) 0.012 Uiso 1 1 d R U . . .
N2 N 0.39853(14) 0.46954(12) 0.75952(9) 0.0113(2) Uani 1 1 d . . . . .
N3 N 0.35398(14) 0.34479(12) 0.92395(9) 0.0105(2) Uani 1 1 d . . . . .
C1 C 0.05422(16) 0.33648(14) 0.77403(10) 0.0115(2) Uani 1 1 d . . . . .
H1A H -0.0014(7) 0.3654(4) 0.7086(8) 0.014 Uiso 1 1 calc R U . . .
H1B H -0.0283(11) 0.2854(7) 0.8144(5) 0.014 Uiso 1 1 calc R U . . .
C2 C 0.37731(17) 0.34949(14) 0.68760(10) 0.0124(2) Uani 1 1 d . . . . .
H2A H 0.4864(14) 0.3068(6) 0.67611(19) 0.015 Uiso 1 1 calc R U . . .
H2B H 0.3301(6) 0.3800(4) 0.6210(9) 0.015 Uiso 1 1 calc R U . . .
C3 C 0.32790(17) 0.20468(14) 0.87759(10) 0.0114(2) Uani 1 1 d . . . . .
H3A H 0.2525(10) 0.1506(7) 0.9205(6) 0.014 Uiso 1 1 calc R U . . .
H3B H 0.4360(14) 0.1564(6) 0.87430(11) 0.014 Uiso 1 1 calc R U . . .
C4 C 0.24214(17) 0.54469(14) 0.77274(10) 0.0124(2) Uani 1 1 d . . . . .
H4A H 0.1936(7) 0.5667(3) 0.7060(9) 0.015 Uiso 1 1 calc R U . . .
H4B H 0.2663(4) 0.6291(12) 0.8082(5) 0.015 Uiso 1 1 calc R U . . .
C5 C 0.47107(17) 0.42927(15) 0.86259(10) 0.0124(2) Uani 1 1 d . . . . .
H5A H 0.5002(4) 0.5116(11) 0.9014(5) 0.015 Uiso 1 1 calc R U . . .
H5B H 0.5741(14) 0.3778(7) 0.85280(16) 0.015 Uiso 1 1 calc R U . . .
C6 C 0.19760(17) 0.41912(14) 0.93907(10) 0.0111(2) Uani 1 1 d . . . . .
H6A H 0.2208(3) 0.5006(11) 0.9805(6) 0.013 Uiso 1 1 calc R U . . .
H6B H 0.1204(10) 0.3615(8) 0.9767(5) 0.013 Uiso 1 1 calc R 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'
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'
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
O1 P1 C1 112.40(6) . . ?
O1 P1 C3 119.29(6) . . ?
C1 P1 C3 100.60(6) . . ?
O1 P1 C2 118.37(6) . . ?
C1 P1 C2 100.61(6) . . ?
C3 P1 C2 102.62(6) . . ?
C1 N1 C4 110.92(10) . . ?
C1 N1 C6 110.72(10) . . ?
C4 N1 C6 108.66(10) . . ?
C1 N1 H1 108.8 . . ?
C4 N1 H1 108.7 . . ?
C6 N1 H1 109.0 . . ?
C4 N2 C5 109.69(10) . . ?
C4 N2 C2 112.59(11) . . ?
C5 N2 C2 112.47(11) . . ?
C6 N3 C5 110.14(11) . . ?
C6 N3 C3 113.43(10) . . ?
C5 N3 C3 111.81(10) . . ?
N1 C1 P1 109.83(8) . . ?
N1 C1 H1A 109.7 . . ?
P1 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
P1 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 P1 108.35(9) . . ?
N2 C2 H2A 110.0 . . ?
P1 C2 H2A 110.0 . . ?
N2 C2 H2B 110.0 . . ?
P1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
N3 C3 P1 108.33(9) . . ?
N3 C3 H3A 110.0 . . ?
P1 C3 H3A 110.0 . . ?
N3 C3 H3B 110.0 . . ?
P1 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
N2 C4 N1 112.03(11) . . ?
N2 C4 H4A 109.2 . . ?
N1 C4 H4A 109.2 . . ?
N2 C4 H4B 109.2 . . ?
N1 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N2 C5 N3 113.04(10) . . ?
N2 C5 H5A 109.0 . . ?
N3 C5 H5A 109.0 . . ?
N2 C5 H5B 109.0 . . ?
N3 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
N3 C6 N1 111.28(10) . . ?
N3 C6 H6A 109.4 . . ?
N1 C6 H6A 109.4 . . ?
N3 C6 H6B 109.4 . . ?
N1 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
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 O1 1.4931(10) . ?
P1 C1 1.8175(13) . ?
P1 C3 1.8160(14) . ?
P1 C2 1.8184(14) . ?
N1 C1 1.5005(17) . ?
N1 C4 1.5233(17) . ?
N1 C6 1.5288(17) . ?
N1 H1 0.897(18) . ?
N2 C4 1.4393(17) . ?
N2 C5 1.4719(17) . ?
N2 C2 1.4841(18) . ?
N3 C6 1.4390(17) . ?
N3 C5 1.4710(17) . ?
N3 C3 1.4864(17) . ?
C1 H1A 0.973(12) . ?
C1 H1B 0.973(12) . ?
C2 H2A 0.965(13) . ?
C2 H2B 0.965(13) . ?
C3 H3A 0.970(13) . ?
C3 H3B 0.970(13) . ?
C4 H4A 0.948(13) . ?
C4 H4B 0.948(13) . ?
C5 H5A 0.960(13) . ?
C5 H5B 0.960(13) . ?
C6 H6A 0.962(13) . ?
C6 H6B 0.962(13) . ?
