Covalent and ionic bonding in bi- and tricyclic Group 15 amides: equidistant P-I and As-I bonds and fluxional cations.
Musongong, Joseph T.; Otang, Mathew E.; Mash, Brandon L.; Zeller, Matthias; Stahl, Lothar; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6341–6354; doi:10.1039/d0dt01163k

data_7704238
_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 P2 Sb'
_chemical_formula_sum            'C16 H36 I N4 P2 Sb'
_chemical_formula_weight         595.10
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_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                 93.325(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.6060(6)
_cell_length_b                   18.7374(12)
_cell_length_c                   26.7135(18)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.536
_cell_measurement_theta_min      2.304
_cell_volume                     4800.1(5)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9908
_diffrn_measured_fraction_theta_max 0.9908
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest Photon100 CMOS'
_diffrn_measurement_method       '\w and \f 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  0.0482
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68044
_diffrn_reflns_theta_full        30.5841
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         2.30
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.576
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1060 before and 0.0587 after correction. The Ratio of minimum to maximum transmission is 0.6581. The \l/2 correction factor is Not present.'
_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    1.6468
_exptl_crystal_description       needle
_exptl_crystal_F_000             2346.0371
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.8898
_refine_diff_density_min         -1.4551
_refine_diff_density_rms         0.2126
_refine_ls_d_res_high            0.6984
_refine_ls_d_res_low             8.8391
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    96
_refine_ls_number_parameters     458
_refine_ls_number_reflns         14615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0235
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+8.1471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                11523
_reflns_number_total             14615
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt01163k2.cif
_cod_data_source_block           J_MUS_15_CPTSbI_0m
_cod_depositor_comments
'Adding full bibliography for 7704230--7704239.cif.'
_cod_database_code               7704238
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C42B(H42a,H42b,H42c), C41B(H41a,H41b,H41c), C43B(H43a,H43b,H43c), C11B(H11a,
 H11b,H11c), C21A(H21d,H21e,H21f), C22A(H22d,H22e,H22f), C23A(H23d,H23e,H23f),
 C21B(H21a,H21b,H21c), C22B(H22a,H22b,H22c), C33A(H33d,H33e,H33f), C31A(H31d,
 H31e,H31f), C32A(H32d,H32e,H32f), C11A(H11d,H11e,H11f), C13A(H13d,H13e,H13f),
 C12A(H12d,H12e,H12f), C42A(H42d,H42e,H42f), C41A(H41d,H41e,H41f), C43A(H43d,
 H43e,H43f), C12B(H12a,H12b,H12c), C13B(H13a,H13b,H13c), C32B(H32a,H32b,H32c),
 C31B(H31a,H31b,H31c), C23B(H23a,H23b,H23c), C33B(H33a,H33b,H33c)
;
_olex2_submission_special_instructions 'No special instructions were received'