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_7704233
_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_absolute_configuration unk
_chemical_formula_moiety         'C28 H46 Cl2 N4 P4'
_chemical_formula_sum            'C28 H46 Cl2 N4 P4'
_chemical_formula_weight         633.50
_chemical_melting_point          428.0(10)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     iterative
_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                 114.4860(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8985(6)
_cell_length_b                   16.8686(10)
_cell_length_c                   11.0098(6)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    150
_cell_measurement_theta_max      33.182
_cell_measurement_theta_min      2.365
_cell_volume                     1673.01(17)
_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      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 0.9625
_diffrn_measured_fraction_theta_max 0.9625
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32695
_diffrn_reflns_theta_full        33.2335
_diffrn_reflns_theta_max         33.23
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0492 before and 0.0452 after correction. The Ratio of minimum to maximum transmission is 0.9423. The \l/2 correction factor is Not present.'
_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    1.2575
_exptl_crystal_description       plate
_exptl_crystal_F_000             673.5818
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/THF'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.3373
_refine_diff_density_min         -0.4547
_refine_diff_density_rms         0.0830
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_d_res_high            0.6484
_refine_ls_d_res_low             9.0083
_refine_ls_goodness_of_fit_ref   1.0314
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     355
_refine_ls_number_reflns         12362
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0314
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0436P)^2^+0.0588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.931
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_gt                11204
_reflns_number_total             12362
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt01163k2.cif
_cod_data_source_block           J_MUS_04_CPTP2Ph2Cl2_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '427-429' was changed to
'428.0(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 2yb'
_cod_database_code               7704233
_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:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C56(H56), C55(H55), C54(H54),
 C53(H53), C52(H52)
2.b Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C31(H31a,H31b,H31c), C22(H22a,H22b,
 H22c), C23(H23a,H23b,H23c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C41(H41a,
 H41b,H41c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c),
 C21(H21a,H21b,H21c)
;
_olex2_submission_original_sample_id (1ab)2
_olex2_submission_special_instructions 'No special instructions were received'