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_7717878
_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         'C36 H62 N6 O4 P4'
_chemical_formula_sum            'C36 H62 N6 O4 P4'
_chemical_formula_weight         766.79
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2lnyv2
_audit_creation_date             2024-11-18
_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                74.121(5)
_cell_angle_beta                 82.724(5)
_cell_angle_gamma                83.213(5)
_cell_formula_units_Z            1
_cell_length_a                   9.4064(5)
_cell_length_b                   9.6314(6)
_cell_length_c                   12.6177(7)
_cell_measurement_reflns_used    3136
_cell_measurement_temperature    250.01(10)
_cell_measurement_theta_max      22.5420
_cell_measurement_theta_min      2.8530
_cell_volume                     1086.46(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -69.00 119.00   0.50   20.00    --   29.89  54.00  80.00  376
  2  \w    -69.00 119.00   0.50   20.00    --   29.89  54.00-150.00  376
  3  \w    -69.00 119.00   0.50   20.00    --   29.89  54.00-180.00  376
  4  \w    -69.00 119.00   0.50   20.00    --   29.89  54.00-150.00  376
  5  \w    -69.00 -17.50   0.50   20.00    --   29.89  54.00 -30.00  103
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0403862000
_diffrn_orient_matrix_UB_12      0.0169871000
_diffrn_orient_matrix_UB_13      0.0469325000
_diffrn_orient_matrix_UB_21      0.0397722000
_diffrn_orient_matrix_UB_22      0.0607519000
_diffrn_orient_matrix_UB_23      -0.0077312000
_diffrn_orient_matrix_UB_31      -0.0510938000
_diffrn_orient_matrix_UB_32      0.0439131000
_diffrn_orient_matrix_UB_33      -0.0344530000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13771
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.054
_diffrn_reflns_theta_min         2.630
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0813
_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^)+(0.1190P)^2^+1.4852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2108
_refine_ls_wR_factor_ref         0.2518
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2634
_reflns_number_total             3838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03229b2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7717876--7717880.cif.'
_cod_database_code               7717878
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C3A) = Uanis(C4) = Uanis(C4A) = Uanis(C2) = Uanis(C2A) = Uanis(C3)
Uanis(C7) = Uanis(C8) = Uanis(C6)
2. Others
 Fixed Sof: C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5)
 H3AC(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5)
 H4AC(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C18(H18), C15(H15), C17(H17), C16(H16)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C3(H3A,
 H3B,H3C), C4(H4A,H4B,H4C), C3A(H3AA,H3AB,H3AC), C2A(H2AA,H2AB,H2AC), C4A(H4AA,
 H4AB,H4AC)
;
_shelx_res_checksum              3119
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.435
_oxdiff_exptl_absorpt_empirical_full_min 0.815