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_7717877
_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         'C26 H76 B6 N6 O4 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C28 H80 B6 Cl4 N6 O4 P4'
_chemical_formula_weight         895.52
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-19
_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                 93.963(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4889(7)
_cell_length_b                   17.3728(11)
_cell_length_c                   16.2634(10)
_cell_measurement_reflns_used    2125
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7310
_cell_measurement_theta_min      2.6420
_cell_volume                     2674.6(3)
_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_temperature      293(2)
_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    -69.00 118.20   0.30   15.00    --   29.89  54.00 -90.00  624
  2  \w    -69.00 118.20   0.30   15.00    --   29.89  54.00  60.00  624
  3  \w    -69.00  10.20   0.30   15.00    --   29.89  54.00 150.00  264
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  Compound_9
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0571171000
_diffrn_orient_matrix_UB_12      0.0246344000
_diffrn_orient_matrix_UB_13      0.0080287000
_diffrn_orient_matrix_UB_21      0.0058113000
_diffrn_orient_matrix_UB_22      0.0182987000
_diffrn_orient_matrix_UB_23      -0.0385996000
_diffrn_orient_matrix_UB_31      -0.0481454000
_diffrn_orient_matrix_UB_32      -0.0269535000
_diffrn_orient_matrix_UB_33      -0.0188529000
_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  0.0633
_diffrn_reflns_av_unetI/netI     0.0530
_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       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19466
_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         25.050
_diffrn_reflns_theta_min         2.450
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64131
_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            'whiteish pink'
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.655
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4738
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0801
_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^)+(0.1369P)^2^+3.5433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2126
_refine_ls_wR_factor_ref         0.2466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3367
_reflns_number_total             4738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03229b2.cif
_cod_data_source_block           Compound_9
_cod_depositor_comments
'Adding full bibliography for 7717876--7717880.cif.'
_cod_database_code               7717877
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Shared sites
{Cl1A, Cl1B}
{Cl3A, Cl3B}
2. Uiso/Uaniso restraints and constraints
Uanis(Cl3A) \\sim Ueq, Uanis(Cl3B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Cl1A) = Uanis(Cl1B)
Uanis(Cl3B) = Uanis(Cl3A)
Uanis(C14) = Uanis(C14A)
Uanis(C5) = Uanis(C14A) = Uanis(C14)
3. Others
 Sof(Cl1B)=Sof(Cl3B)=Sof(C14)=Sof(H14A)=Sof(H14B)=1-FVAR(1)
 Sof(Cl1A)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(Cl3A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C9(H9A,H9B), C14(H14A,H14B),
 C14A(H14C,H14D)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C1(H1A,H1B,H1C),
 C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93503
_shelx_fab_checksum              9143
_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 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.835