Reactions of chalcogens and borane with phosphazane macrocycles assembled from diethanolamine and P<sub>2</sub>N<sub>2</sub> building blocks.
Goyal, Manu; Negi, Chandrakala; Garg, Nitish Kumar; Jain, Shalender; Singh, Sanjay; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4089–4095; doi:10.1039/d4dt03229b

data_7717880
_publ_section_title
;
 Reactions of chalcogens and borane with phosphazane macrocycles assembled
 from diethanolamine and P<sub>2</sub>N<sub>2</sub> building blocks.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4089
_journal_page_last               4095
_journal_paper_doi               10.1039/d4dt03229b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'2(C7 H5 Cl O2), 2(C13 H29 N3 O4 P2), 2(C4 H8 O)'
_chemical_formula_sum            'C48 H84 Cl2 N6 O14 P4'
_chemical_formula_weight         1163.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-12-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-20 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                94.818(4)
_cell_angle_beta                 99.230(4)
_cell_angle_gamma                115.342(4)
_cell_formula_units_Z            2
_cell_length_a                   14.2255(7)
_cell_length_b                   15.0529(7)
_cell_length_c                   15.8213(8)
_cell_measurement_reflns_used    6305
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      24.5240
_cell_measurement_theta_min      2.6460
_cell_volume                     2977.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      99.99(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00 118.20   0.30   10.00    --   29.89  54.00  63.00  624
  2  \w    -69.00 118.20   0.30   10.00    --   29.89  54.00-150.00  624
  3  \w    -69.00 118.20   0.30   10.00    --   29.89  54.00   0.00  624
  4  \w    -64.00 118.10   0.30   10.00    --   29.89  54.00 -60.00  607
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'compound 3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36012
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.054
_diffrn_reflns_theta_max         25.054
_diffrn_reflns_theta_min         2.648
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.120
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         10511
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1304P)^2^+3.5108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7499
_reflns_number_total             10511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03229b2.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
'Adding full bibliography for 7717876--7717880.cif.'
_cod_database_code               7717880
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Restrained distances
 C34-C32
 1.45 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C32) =
Uanis(C34)
Uanis(O10) = Uanis(O9)
Uanis(O15) = Uanis(O49)
3. Others
 Sof(H31C)=Sof(H31D)=Sof(H34C)=Sof(H34D)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(O49)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=1-FVAR(1)
 Sof(H31A)=Sof(H31B)=Sof(H34A)=Sof(H34B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(O15)=
 Sof(C49)=Sof(H49A)=Sof(H49B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C18(H18A,H18B), C19(H19A,
 H19B), C21(H21A,H21B), C22(H22A,H22B), C27(H27A,H27B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31C,H31D), C31(H31A,H31B), C34(H34A,H34B),
  C34(H34C,H34D), C32(H32A,H32B), C33(H33A,H33B), C16(H16A,H16B), C49(H49A,H49B)
4.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C44(H44), C45(H45), C48(H48), C36(H36), C37(H37), C38(H38), C41(H41)
4.c Tetrahedral OH refined with riding coordinates:
 O10(H10), O12(H12)
4.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C),
 C50(H50A,H50B,H50C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              57989
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;