#------------------------------------------------------------------------------
#$Date: 2020-06-05 13:42:38 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252767 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/42/7704237.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_7704237
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 As I N4 P2'
_chemical_formula_sum            'C16 H36 As I N4 P2'
_chemical_formula_weight         548.26
_chemical_melting_point          460.0(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             2020-03-17
_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                 96.533(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5274(8)
_cell_length_b                   11.9897(9)
_cell_length_c                   10.3478(7)
_cell_measurement_reflns_used    9007
_cell_measurement_temperature    150
_cell_measurement_theta_max      33.214
_cell_measurement_theta_min      2.742
_cell_volume                     1174.36(15)
_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 0.9964
_diffrn_measured_fraction_theta_max 0.9964
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0196
_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            28533
_diffrn_reflns_theta_full        33.2342
_diffrn_reflns_theta_max         33.23
_diffrn_reflns_theta_min         2.61
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.904
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1152 before and 0.0423 after correction. The Ratio of minimum to maximum transmission is 0.6549. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'dull yellowish yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.5504
_exptl_crystal_description       plate
_exptl_crystal_F_000             551.8509
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.2625
_refine_diff_density_min         -0.8886
_refine_diff_density_rms         0.1008
_refine_ls_d_res_high            0.6484
_refine_ls_d_res_low             7.8044
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     127
_refine_ls_number_reflns         4681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0219
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0118P)²+1.1000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0493
_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                4112
_reflns_number_total             4681
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt01163k2.cif
_cod_data_source_block           J_MUS_02_CPTAsI_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '459-461' was changed to
'460.0(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               7704237
_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) H21b(0.5) H21c(0.5)
3.a Me refined with riding coordinates:
 C11(H11a,H11b,H11c), C21(H21a,H21b,H21c)
3.b Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C12(H12a,H12b,H12c), C22(H22a,H22b,
 H22c), C31(H31a,H31b,H31c)
;
_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 0.862430(17) 0.25 0.518786(12) 0.02999(5) Uani 1.000000 2 S T P .
N3 N 0.78668(11) 0.13062(8) 0.19924(10) 0.01518(18) Uani 1.000000 1 . . . .
As1 As 0.895863(18) 0.25 0.259529(17) 0.01512(5) Uani 1.000000 2 S T P .
C10 C 0.6730(2) 0.25 -0.09989(17) 0.0188(3) Uani 1.000000 2 S T P .
N2 N 0.56242(16) 0.25 0.23652(15) 0.0172(3) Uani 1.000000 2 S T P .
P1 P 0.61094(3) 0.14372(3) 0.13851(3) 0.01578(6) Uani 1.000000 1 . . . .
N1 N 0.61708(16) 0.25 0.02785(14) 0.0163(3) Uani 1.000000 2 S T P .
C32 C 0.81764(18) -0.05599(12) 0.10464(15) 0.0293(3) Uani 1.000000 1 . . . .
H32a H 0.7156(2) -0.0598(9) 0.0783(7) 0.0439(4) Uiso 1.000000 1 GR . . .
H32b H 0.8644(12) -0.0225(6) 0.0345(4) 0.0439(4) Uiso 1.000000 1 GR . . .
H32c H 0.8547(12) -0.1314(3) 0.1225(4) 0.0439(4) Uiso 1.000000 1 GR . . .
C33 C 0.77574(17) -0.03792(12) 0.33863(15) 0.0266(3) Uani 1.000000 1 . . . .
H33a H 0.7930(11) 0.0086(6) 0.4167(4) 0.0399(4) Uiso 1.000000 1 GR . . .
H33b H 0.6738(2) -0.0441(10) 0.3131(5) 0.0399(4) Uiso 1.000000 1 GR . . .
H33c H 0.8155(10) -0.1124(4) 0.3571(8) 0.0399(4) Uiso 1.000000 1 GR . . .
C11 C 0.8341(2) 0.25 -0.08883(19) 0.0240(4) Uani 1.000000 2 S T P .
H11a H 0.8647(2) 0.25 -0.17609(19) 0.0360(6) Uiso 1.000000 2 RS T P -1
H11b H 0.8705(2) 0.31673783742 -0.04165(19) 0.0360(6) Uiso 0.500000 1 R . . -1
H11c H 0.8705(2) 0.18326216258 -0.04165(19) 0.0360(6) Uiso 0.500000 1 R . . -1
C12 C 0.6181(2) 0.14573(16) -0.17273(16) 0.0390(4) Uani 1.000000 1 . . . .
H12a H 0.6527(13) 0.07944(16) -0.1236(7) 0.0585(6) Uiso 1.000000 1 GR . . .
H12b H 0.5146(2) 0.1461(6) -0.1827(13) 0.0585(6) Uiso 1.000000 1 GR . . .
H12c H 0.6517(13) 0.1445(6) -0.2588(6) 0.0585(6) Uiso 1.000000 1 GR . . .
C20 C 0.4350(2) 0.25 0.3061(2) 0.0246(4) Uani 1.000000 2 S T P .
C22 C 0.4402(2) 0.35417(15) 0.39130(18) 0.0394(4) Uani 1.000000 1 . . . .
H22a H 0.5280(7) 0.3543(6) 0.4507(10) 0.0590(6) Uiso 1.000000 1 GR . . .
H22b H 0.4368(16) 0.42077(15) 0.33611(19) 0.0590(6) Uiso 1.000000 1 GR . . .
H22c H 0.3593(9) 0.3543(6) 0.4418(11) 0.0590(6) Uiso 1.000000 1 GR . . .
C21 C 0.3021(2) 0.25 0.2095(3) 0.0453(7) Uani 1.000000 2 S T P .
H21a H 0.2187(2) 0.25 0.2568(3) 0.0679(10) Uiso 1.000000 2 RS T P -1
H21b H 0.3010(2) 0.31673783742 0.1547(3) 0.0679(10) Uiso 0.500000 1 R . . -1
H21c H 0.3010(2) 0.18326216258 0.1547(3) 0.0679(10) Uiso 0.500000 1 R . . -1
C31 C 1.00561(15) 0.02118(13) 0.26570(16) 0.0278(3) Uani 1.000000 1 . . . .
H31a H 1.0505(2) 0.0569(9) 0.1958(5) 0.0417(4) Uiso 1.000000 1 GR . . .
H31b H 1.02547(16) 0.0647(9) 0.3458(7) 0.0417(4) Uiso 1.000000 1 GR . . .
H31c H 1.0432(2) -0.05445(14) 0.2800(12) 0.0417(4) Uiso 1.000000 1 GR . . .
C30 C 0.84606(14) 0.01545(11) 0.22753(13) 0.0196(2) Uani 1.000000 1 . . . .
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
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'
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'
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'
As 0.07000 2.09310 16.67230 6.07010 3.43130 4.27790 2.63450 0.26470 12.94790
47.79720 2.53099989891
'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
P1 N3 As1 122.75(6) . . ?
C30 N3 As1 117.52(8) . . ?
C30 N3 P1 118.72(8) . . ?
N3 As1 I1 102.03(3) . . ?
N3 As1 I1 102.03(3) 4_565 . ?
N3 As1 N3 102.41(6) 4_565 . ?
C11 C10 N1 113.22(15) . . ?
C12 C10 N1 107.69(11) 4_565 . ?
C12 C10 N1 107.69(11) . . ?
C12 C10 C11 108.87(12) 4_565 . ?
C12 C10 C11 108.87(12) . . ?
C12 C10 C12 110.50(19) 4_565 . ?
P1 N2 P1 95.31(7) 4_565 . ?
C20 N2 P1 125.14(7) . 4_565 ?
C20 N2 P1 125.14(7) . . ?
N2 P1 N3 99.61(6) . . ?
P1 P1 N3 95.22(4) 4_565 . ?
P1 P1 N2 42.35(4) 4_565 . ?
N1 P1 N3 101.81(6) . . ?
N1 P1 N2 82.86(5) . . ?
P1 N1 C10 129.64(5) . . ?
P1 N1 C10 129.64(5) 4_565 . ?
P1 N1 P1 95.71(7) 4_565 . ?
C22 C20 N2 107.82(11) . . ?
C22 C20 N2 107.82(11) 4_565 . ?
C22 C20 C22 109.82(19) . 4_565 ?
C21 C20 N2 110.37(18) . . ?
C21 C20 C22 110.47(13) . 4_565 ?
C21 C20 C22 110.47(13) . . ?
C32 C30 N3 108.90(11) . . ?
C33 C30 N3 109.94(10) . . ?
C33 C30 C32 109.74(12) . . ?
C31 C30 N3 110.44(11) . . ?
C31 C30 C32 108.45(12) . . ?
C31 C30 C33 109.35(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
I1 As1 2.7373(3) . ?
N3 As1 1.8364(10) . ?
N3 P1 1.7273(11) . ?
N3 C30 1.5083(16) . ?
C10 N1 1.480(2) . ?
C10 C11 1.525(3) . ?
C10 C12 1.5214(19) . ?
C10 C12 1.5214(19) 4_565 ?
N2 P1 1.7242(10) 4_565 ?
N2 P1 1.7242(10) . ?
N2 C20 1.480(2) . ?
P1 P1 2.5486(7) 4_565 ?
P1 N1 1.7187(10) . ?
C32 C30 1.532(2) . ?
C33 C30 1.5347(18) . ?
C20 C22 1.526(2) . ?
C20 C22 1.526(2) 4_565 ?
C20 C21 1.521(3) . ?
C31 C30 1.528(2) . ?
