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_7717879
_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 Se4, 2(C6 D6)'
_chemical_formula_sum            'C48 H62 D12 N6 O4 P4 Se4'
_chemical_formula_weight         1250.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                90
_cell_angle_beta                 111.913(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0929(8)
_cell_length_b                   13.8043(7)
_cell_length_c                   16.9771(13)
_cell_measurement_reflns_used    2507
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      24.8610
_cell_measurement_theta_min      2.8690
_cell_volume                     2846.7(4)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200.00(10)
_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    -69.00 118.20   0.30   20.00    --   29.89  54.00-180.00  624
  2  \w    -69.00 -24.60   0.30   20.00    --   29.89  54.00  30.00  148
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'Compound 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10513
_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         25.047
_diffrn_reflns_theta_min         2.503
_exptl_absorpt_coefficient_mu    2.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94761
_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    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.547
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0778P)^2^+2.1284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3934
_reflns_number_total             5045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03229b2.cif
_cod_data_source_block           compound_8
_cod_depositor_comments
'Adding full bibliography for 7717876--7717880.cif.'
_cod_original_cell_volume        2846.7(3)
_cod_database_code               7717879
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C23) = Uanis(C22) = Uanis(C21) = Uanis(C20) = Uanis(C19)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C18(H18), C16(H16), C17(H17), C24(D24), C19(D19),
 C21(D21), C23(D23), C22(D22), C20(D20)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C2(H2A,H2B,
 H2C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              78176
_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
;