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_7704235
_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         'C22 H41 N4 P2 Sb'
_chemical_formula_sum            'C22 H41 N4 P2 Sb'
_chemical_formula_weight         545.31
_chemical_melting_point          436.0(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             2019-02-25
_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                 110.3634(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0318(6)
_cell_length_b                   9.6090(4)
_cell_length_c                   18.2097(7)
_cell_measurement_reflns_used    9719
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      37.67
_cell_measurement_theta_min      2.30
_cell_volume                     2629.88(18)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9601
_diffrn_measured_fraction_theta_max 0.9468
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36559
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         33.00
_diffrn_reflns_theta_min         2.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_type   none
_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    1.3771
_exptl_crystal_description       block
_exptl_crystal_F_000             1126.6618
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.74
_exptl_crystal_size_min          0.67
_refine_diff_density_max         0.5248
_refine_diff_density_min         -0.7472
_refine_diff_density_rms         0.0820
_refine_ls_d_res_high            0.6525
_refine_ls_d_res_low             8.0959
_refine_ls_goodness_of_fit_ref   1.0312
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    58
_refine_ls_number_parameters     274
_refine_ls_number_reflns         9401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0312
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+1.8489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -24
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -14
_reflns_number_gt                8743
_reflns_number_total             9401
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt01163k2.cif
_cod_data_source_block           MAT41_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '435-437' was changed to
'436.0(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               7704235
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
2.b 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'