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_7704239
_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         'C17 H36 F3 N4 O3 P2 S Sb'
_chemical_formula_sum            'C17 H36 F3 N4 O3 P2 S Sb'
_chemical_formula_weight         617.27
_chemical_melting_point          430.0(10)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 100.5301(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7212(3)
_cell_length_b                   18.6010(5)
_cell_length_c                   15.2849(4)
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.99
_cell_measurement_theta_min      2.40
_cell_volume                     2717.33(13)
_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      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.9922
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49097
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         38.00
_diffrn_reflns_theta_min         2.40
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.254
_exptl_absorpt_correction_T_max  0.612
_exptl_absorpt_correction_T_min  0.420
_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    1.5087
_exptl_crystal_description       needle
_exptl_crystal_F_000             1255.4459
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.39
_refine_diff_density_max         2.3216
_refine_diff_density_min         -1.8374
_refine_diff_density_rms         0.1856
_refine_ls_d_res_high            0.5771
_refine_ls_d_res_low             8.5010
_refine_ls_goodness_of_fit_ref   1.0568
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     292
_refine_ls_number_reflns         14692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0568
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.7969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -16
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -12
_reflns_number_gt                12760
_reflns_number_total             14692
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt01163k2.cif
_cod_data_source_block           MAT45_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '429-431' was changed to
'430.0(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_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7704239
_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:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C21(H21a,H21b,
 H21c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C31(H31a,H31b,H31c), C32(H32a,
 H32b,H32c), C33(H33a,H33b,H33c), C41(H41a,H41b,H41c), C42(H42a,H42b,H42c),
 C43(H43a,H43b,H43c)
;
_olex2_submission_special_instructions 'No special instructions were received'