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_7704236
_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       '\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  0.0261
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0150P)^2^+0.5951P] where P=(Fo^2^+2Fc^2^)/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'