#------------------------------------------------------------------------------
#$Date: 2020-06-05 12:42:38 +0200 (vie 05 de jun de 2020) $
#$Revision: 252767 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/42/7704236.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_7704236
loop_
_publ_author_name
'Musongong, Joseph T.'
'Otang, Mathew E.'
'Mash, Brandon L.'
'Zeller, Matthias'
'Stahl, Lothar'
_publ_section_title
;
 Covalent and ionic bonding in bi- and tricyclic Group 15 amides:
 equidistant P-I and As-I bonds and fluxional cations.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6341
_journal_page_last               6354
_journal_paper_doi               10.1039/d0dt01163k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C16 H36 I N4 P3'
_chemical_formula_sum            'C16 H36 I N4 P3'
_chemical_formula_weight         504.32
_chemical_melting_point          486.0(10)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_Int_Tables_number      11
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.573(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5405(7)
_cell_length_b                   11.8694(8)
_cell_length_c                   10.3274(7)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    150
_cell_measurement_theta_max      33.203
_cell_measurement_theta_min      2.626
_cell_volume                     1161.79(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9944
_diffrn_measured_fraction_theta_max 0.9940
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest Photon100 CMOS'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26788
_diffrn_reflns_theta_full        33.2216
_diffrn_reflns_theta_max         33.22
_diffrn_reflns_theta_min         2.62
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.591
_exptl_absorpt_correction_T_max  0.564
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4415
_exptl_crystal_description       cube
_exptl_crystal_F_000             515.9084
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.6691
_refine_diff_density_min         -0.7073
_refine_diff_density_rms         0.0709
_refine_ls_d_res_high            0.6486
_refine_ls_d_res_low             7.7618
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0401
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     127
_refine_ls_number_reflns         4626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0401
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0150P)²+0.5951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0452
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4262
_reflns_number_total             4626
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt01163k2.cif
_cod_data_source_block           J_MUS_01_CPTPI_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '485-487' was changed to
'486.0(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7704230--7704239.cif.
;
_cod_database_code               7704236
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H11b(0.5) H11c(0.5) H22b(0.5) H22c(0.5)
3.a Me refined with riding coordinates:
 C11(H11a,H11b,H11c), C22(H22a,H22b,H22c)
3.b Idealised Me refined as rotating group:
 C23(H23b,H23c,H23a), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C13(H13c,H13a,
 H13b), C31(H31a,H31b,H31c)
;
_olex2_submission_original_sample_id 1h
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z
3 -x,-y,-z
4 x,-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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
I1 I 0.857105(12) 0.25 0.519890(9) 0.02682(4) Uani 1.000000 2 S T P .
C23 C 0.43431(15) 0.35530(11) 0.39128(14) 0.0361(3) Uani 1.000000 1 . . . .
H23b H 0.3512(6) 0.3563(5) 0.4390(9) 0.0541(4) Uiso 1.000000 1 GR . . .
H23c H 0.5200(6) 0.3547(5) 0.4534(7) 0.0541(4) Uiso 1.000000 1 GR . . .
H23a H 0.4339(12) 0.42251(11) 0.33613(17) 0.0541(4) Uiso 1.000000 1 GR . . .
N3 N 0.78975(8) 0.13806(6) 0.20452(7) 0.01354(13) Uani 1.000000 1 . . . .
P1 P 0.88636(3) 0.25 0.25961(3) 0.01382(6) Uani 1.000000 2 S T P .
N1 N 0.61357(11) 0.25 0.02921(11) 0.01455(19) Uani 1.000000 2 S T P .
C30 C 0.85258(10) 0.02174(8) 0.23096(9) 0.01738(16) Uani 1.000000 1 . . . .
P2 P 0.61122(2) 0.14369(2) 0.14195(2) 0.01413(5) Uani 1.000000 1 . . . .
N2 N 0.56001(12) 0.25 0.23893(11) 0.01576(19) Uani 1.000000 2 S T P .
C32 C 0.82691(12) -0.04873(9) 0.10629(11) 0.0252(2) Uani 1.000000 1 . . . .
H32a H 0.72524(13) -0.0547(7) 0.0797(5) 0.0378(3) Uiso 1.000000 1 GR . . .
H32b H 0.8723(9) -0.0124(4) 0.0368(3) 0.0378(3) Uiso 1.000000 1 GR . . .
H32c H 0.8667(9) -0.1242(3) 0.1226(3) 0.0378(3) Uiso 1.000000 1 GR . . .
C33 C 0.78195(12) -0.03488(9) 0.34007(11) 0.02379(19) Uani 1.000000 1 . . . .
H33a H 0.7979(9) 0.0108(4) 0.4194(3) 0.0357(3) Uiso 1.000000 1 GR . . .
H33b H 0.6804(2) -0.0416(8) 0.3134(4) 0.0357(3) Uiso 1.000000 1 GR . . .
H33c H 0.8225(7) -0.1100(3) 0.3571(7) 0.0357(3) Uiso 1.000000 1 GR . . .
C10 C 0.66918(14) 0.25 -0.09890(13) 0.0174(2) Uani 1.000000 2 S T P .
C11 C 0.83054(15) 0.25 -0.08865(14) 0.0225(3) Uani 1.000000 2 S T P .
H11a H 0.86049(15) 0.25 -0.17631(14) 0.0337(4) Uiso 1.000000 2 RS T P -1
H11b H 0.86721(15) 0.317414245818 -0.04154(14) 0.0337(4) Uiso 0.500000 1 R . .
-1
H11c H 0.86721(15) 0.182585754182 -0.04154(14) 0.0337(4) Uiso 0.500000 1 R . .
-1
C13 C 0.61377(15) 0.35537(12) -0.17188(12) 0.0346(3) Uani 1.000000 1 . . . .
H13c H 0.51040(15) 0.3552(5) -0.1809(10) 0.0519(4) Uiso 1.000000 1 GR . . .
H13a H 0.6491(10) 0.42240(12) -0.1232(6) 0.0519(4) Uiso 1.000000 1 GR . . .
H13b H 0.6462(10) 0.3563(5) -0.2585(4) 0.0519(4) Uiso 1.000000 1 GR . . .
C20 C 0.43081(15) 0.25 0.30613(15) 0.0224(3) Uani 1.000000 2 S T P .
C22 C 0.29947(17) 0.25 0.2063(2) 0.0381(4) Uani 1.000000 2 S T P .
H22a H 0.21482(17) 0.25 0.2519(2) 0.0571(6) Uiso 1.000000 2 RS T P -1
H22b H 0.29969(17) 0.317414245818 0.1516(2) 0.0571(6) Uiso 0.500000 1 R . . -1
H22c H 0.29969(17) 0.182585754182 0.1516(2) 0.0571(6) Uiso 0.500000 1 R . . -1
C31 C 1.01204(11) 0.02923(9) 0.27082(12) 0.0254(2) Uani 1.000000 1 . . . .
H31a H 1.05687(17) 0.0667(7) 0.2017(4) 0.0381(3) Uiso 1.000000 1 GR . . .
H31b H 1.03026(12) 0.0726(7) 0.3518(5) 0.0381(3) Uiso 1.000000 1 GR . . .
H31c H 1.0509(2) -0.04681(10) 0.2845(9) 0.0381(3) Uiso 1.000000 1 GR . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
I -0.41187 1.83264 20.14720 18.99490 7.51380 2.27350 4.34700 0.38140 27.76600
66.87760 4.07119989395
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.10434 0.09671 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
C30 N3 P1 117.96(6) . . ?
P2 N3 P1 124.57(5) . . ?
P2 N3 C30 116.64(6) . . ?
N3 P1 I1 102.67(3) 4_565 . ?
N3 P1 I1 102.67(3) . . ?
N3 P1 N3 104.64(5) 4_565 . ?
P2 N1 P2 94.46(6) 4_565 . ?
C10 N1 P2 129.72(4) . . ?
C10 N1 P2 129.72(4) . 4_565 ?
C32 C30 N3 108.90(8) . . ?
C33 C30 N3 109.47(8) . . ?
C33 C30 C32 109.70(8) . . ?
C31 C30 N3 110.80(8) . . ?
C31 C30 C32 108.41(8) . . ?
C31 C30 C33 109.54(8) . . ?
N1 P2 N3 100.97(4) . . ?
P2 P2 N3 92.19(3) 4_565 . ?
P2 P2 N1 42.77(3) 4_565 . ?
N2 P2 N3 98.19(5) . . ?
N2 P2 N1 83.24(4) . . ?
P2 N2 P2 94.64(6) 4_565 . ?
C20 N2 P2 125.50(5) . 4_565 ?
C20 N2 P2 125.50(5) . . ?
C11 C10 N1 113.49(11) . . ?
C13 C10 N1 107.61(8) 4_565 . ?
C13 C10 N1 107.61(8) . . ?
C13 C10 C11 108.87(9) . . ?
C13 C10 C11 108.87(9) 4_565 . ?
C13 C10 C13 110.38(14) . 4_565 ?
C23 C20 C23 109.94(14) . 4_565 ?
N2 C20 C23 107.77(8) . . ?
N2 C20 C23 107.77(8) . 4_565 ?
C22 C20 C23 110.53(9) . 4_565 ?
C22 C20 C23 110.53(9) . . ?
C22 C20 N2 110.23(13) . . ?
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
I1 P1 2.7340(4) . ?
C23 C20 1.5263(15) 4_565 ?
N3 P1 1.6788(8) . ?
N3 C30 1.5174(12) . ?
N3 P2 1.7525(8) . ?
N1 P2 1.7188(8) 4_565 ?
N1 P2 1.7188(8) . ?
N1 C10 1.4808(17) . ?
C30 C32 1.5314(14) . ?
C30 C33 1.5327(14) . ?
C30 C31 1.5324(14) . ?
P2 P2 2.5236(5) 4_565 ?
P2 N2 1.7164(8) . ?
N2 C20 1.4822(17) . ?
C10 C11 1.531(2) . ?
C10 C13 1.5233(14) 4_565 ?
C10 C13 1.5233(14) . ?
C20 C22 1.529(2) . ?
