#------------------------------------------------------------------------------
#$Date: 2020-06-05 13:42:38 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252767 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/42/7704232.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_7704232
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 N7 P2'
_chemical_formula_sum            'C16 H36 As N7 P2'
_chemical_formula_weight         463.38
_chemical_melting_point          374.0(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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-16
_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                 98.442(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6134(5)
_cell_length_b                   11.6759(6)
_cell_length_c                   10.3557(5)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.640
_cell_measurement_theta_min      2.645
_cell_volume                     1149.78(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.97
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16118
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.664
_diffrn_reflns_theta_min         1.988
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_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    1.338
_exptl_crystal_description       irregular
_exptl_crystal_F_000             488
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.42
_refine_diff_density_max         1.920
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         4279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0252
_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/[σ²(Fo²)+(0.0308P)²+0.7093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4111
_reflns_number_total             4279
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01163k2.cif
_cod_data_source_block           joseph5_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '373-375' was changed to
'374.0(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               7704232
_shelx_shelxl_version_number     2014/7
_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   0.547
_shelx_estimated_absorpt_t_min   0.441
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H12B(0.5) H12C(0.5) H22B(0.5) H22C(0.5)
3.a Me refined with riding coordinates:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'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_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
As1 As 0.07266(2) 0.2500 0.25082(2) 0.01350(5) Uani 1 2 d S T P . .
P1 P 0.36892(3) 0.14092(2) 0.34663(3) 0.01059(6) Uani 1 1 d . . . . .
N1 N 0.37242(13) 0.2500 0.45839(12) 0.0105(2) Uani 1 2 d S T P . .
N2 N 0.41108(13) 0.2500 0.24474(12) 0.0119(2) Uani 1 2 d S T P . .
N3 N 0.19251(9) 0.12705(8) 0.29169(9) 0.01185(15) Uani 1 1 d . . . . .
N4 N 0.04851(19) 0.2500 0.05891(16) 0.0265(3) Uani 1 2 d S T P . .
N5 N 0.14590(18) 0.2500 0.00233(13) 0.0192(3) Uani 1 2 d S T P . .
N6 N 0.2370(3) 0.2500 -0.0593(2) 0.0531(7) Uani 1 2 d S T P . .
C10 C 0.33125(15) 0.2500 0.59047(14) 0.0121(2) Uani 1 2 d S T P . .
C12 C 0.17143(17) 0.2500 0.58787(16) 0.0181(3) Uani 1 2 d S T P . .
H12A H 0.1500 0.2500 0.6775 0.027 Uiso 1 2 calc RS T P . .
H12B H 0.1311 0.3185 0.5422 0.027 Uiso 0.5 1 calc R . . . .
H12C H 0.1311 0.1815 0.5422 0.027 Uiso 0.5 1 calc R . . . .
C11 C 0.39242(16) 0.14270(13) 0.66120(13) 0.0277(3) Uani 1 1 d . . . . .
H11A H 0.3534 0.0746 0.6138 0.042 Uiso 1 1 calc GR . . . .
H11B H 0.3683 0.1416 0.7499 0.042 Uiso 1 1 calc GR . . . .
H11C H 0.4949 0.1429 0.6654 0.042 Uiso 1 1 calc GR . . . .
C20 C 0.54807(17) 0.2500 0.19335(17) 0.0188(3) Uani 1 2 d S T P . .
C21 C 0.55392(16) 0.14272(12) 0.10990(15) 0.0275(3) Uani 1 1 d . . . . .
H21A H 0.5493 0.0745 0.1642 0.041 Uiso 1 1 calc GR . . . .
H21B H 0.6420 0.1421 0.0728 0.041 Uiso 1 1 calc GR . . . .
H21C H 0.4742 0.1427 0.0391 0.041 Uiso 1 1 calc GR . . . .
C22 C 0.67166(19) 0.2500 0.3059(2) 0.0322(5) Uani 1 2 d S T P . .
H22A H 0.7606 0.2500 0.2701 0.048 Uiso 1 2 calc RS T P . .
H22B H 0.6666 0.3185 0.3596 0.048 Uiso 0.5 1 calc R . . . .
H22C H 0.6666 0.1815 0.3596 0.048 Uiso 0.5 1 calc R . . . .
C30 C 0.13451(12) 0.00853(9) 0.26231(11) 0.01526(19) Uani 1 1 d . . . . .
C31 C -0.02613(13) 0.01150(12) 0.22813(14) 0.0231(2) Uani 1 1 d . . . . .
H31A H -0.0669 0.0435 0.3016 0.035 Uiso 1 1 calc GR . . . .
H31B H -0.0616 -0.0665 0.2103 0.035 Uiso 1 1 calc GR . . . .
H31C H -0.0526 0.0593 0.1506 0.035 Uiso 1 1 calc GR . . . .
C32 C 0.17196(14) -0.06758(11) 0.38312(13) 0.0219(2) Uani 1 1 d . . . . .
H32A H 0.2743 -0.0699 0.4076 0.033 Uiso 1 1 calc GR . . . .
H32B H 0.1366 -0.1453 0.3634 0.033 Uiso 1 1 calc GR . . . .
H32C H 0.1289 -0.0362 0.4556 0.033 Uiso 1 1 calc GR . . . .
C33 C 0.19828(16) -0.04133(11) 0.14704(13) 0.0242(2) Uani 1 1 d . . . . .
H33A H 0.1754 0.0086 0.0708 0.036 Uiso 1 1 calc GR . . . .
H33B H 0.1595 -0.1179 0.1264 0.036 Uiso 1 1 calc GR . . . .
H33C H 0.3006 -0.0465 0.1703 0.036 Uiso 1 1 calc GR . . . .
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'
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'
As As 0.0499 2.0058 '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
N3 As1 N3 101.75(6) 4_565 . ?
N3 As1 N4 102.02(4) . . ?
N3 As1 N4 102.02(4) 4_565 . ?
N1 P1 P1 42.15(3) . 4_565 ?
N1 P1 N2 83.26(5) . . ?
N2 P1 P1 42.93(3) . 4_565 ?
N3 P1 P1 95.42(3) . 4_565 ?
N3 P1 N1 102.36(5) . . ?
N3 P1 N2 100.08(5) . . ?
P1 N1 P1 95.69(6) 4_565 . ?
C10 N1 P1 129.92(4) . . ?
C10 N1 P1 129.92(4) . 4_565 ?
P1 N2 P1 94.15(6) . 4_565 ?
C20 N2 P1 120.88(7) . 4_565 ?
C20 N2 P1 120.88(7) . . ?
P1 N3 As1 123.69(5) . . ?
C30 N3 As1 117.83(7) . . ?
C30 N3 P1 118.19(7) . . ?
N5 N4 As1 121.29(13) . . ?
N6 N5 N4 176.5(2) . . ?
N1 C10 C12 112.80(12) . . ?
N1 C10 C11 107.91(8) . 4_565 ?
N1 C10 C11 107.91(8) . . ?
C11 C10 C12 108.86(9) 4_565 . ?
C11 C10 C12 108.86(9) . . ?
C11 C10 C11 110.49(16) 4_565 . ?
N2 C20 C21 108.04(10) . 4_565 ?
N2 C20 C21 108.04(10) . . ?
N2 C20 C22 110.75(14) . . ?
C21 C20 C21 110.17(15) 4_565 . ?
C21 C20 C22 109.90(10) . . ?
C21 C20 C22 109.90(10) 4_565 . ?
N3 C30 C31 110.88(9) . . ?
N3 C30 C32 109.39(9) . . ?
N3 C30 C33 109.11(9) . . ?
C31 C30 C32 108.02(10) . . ?
C31 C30 C33 109.44(10) . . ?
C32 C30 C33 110.00(10) . . ?
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
As1 N3 1.8505(9) 4_565 ?
As1 N3 1.8505(9) . ?
As1 N4 1.9668(17) . ?
P1 P1 2.5472(6) 4_565 ?
P1 N1 1.7180(9) . ?
P1 N2 1.7393(9) . ?
P1 N3 1.7154(9) . ?
N1 P1 1.7179(9) 4_565 ?
N1 C10 1.4786(19) . ?
N2 P1 1.7393(9) 4_565 ?
N2 C20 1.4910(19) . ?
N3 C30 1.5061(14) . ?
N4 N5 1.175(2) . ?
N5 N6 1.157(3) . ?
C10 C12 1.533(2) . ?
C10 C11 1.5249(15) . ?
C10 C11 1.5249(16) 4_565 ?
C20 C21 1.5275(17) 4_565 ?
C20 C21 1.5275(17) . ?
C20 C22 1.537(3) . ?
C30 C31 1.5332(17) . ?
C30 C32 1.5337(17) . ?
C30 C33 1.5345(17) . ?
