#------------------------------------------------------------------------------
#$Date: 2025-07-06 18:28:38 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300763 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/78/7717876.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7717876
loop_
_publ_author_name
'Goyal, Manu'
'Negi, Chandrakala'
'Garg, Nitish Kumar'
'Jain, Shalender'
'Singh, Sanjay'
_publ_section_title
;
 Reactions of chalcogens and borane with phosphazane macrocycles assembled
 from diethanolamine and P₂N₂ 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 H58 N6 O4 P4 '
_chemical_formula_sum            'C26 H58 N6 O4 P4'
_chemical_formula_weight         642.66
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-14
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_audit_update_record
;
2024-11-18 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 126.539(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4422(16)
_cell_length_b                   18.041(3)
_cell_length_c                   12.769(2)
_cell_measurement_reflns_used    5963
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.161
_cell_measurement_theta_min      2.685
_cell_volume                     1747.6(5)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7398
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0642 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.7562.
The λ/2 correction factor is 0.0015.
;
_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    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             696.0
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0684P)²+7.9961P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.1919
_reflns_number_gt                2736
_reflns_number_total             3039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt03229b2.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
'Adding full bibliography for 7717876--7717880.cif.'
_cod_original_formula_sum        'C26 H58 N6 O4 P4 '
_cod_database_code               7717876
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.19133(13) 0.31319(6) 0.82640(9) 0.0200(3) Uani 1 1 d . . .
P2 P -0.05492(13) 0.40340(6) 0.66172(9) 0.0210(3) Uani 1 1 d . . .
O1 O 0.3086(3) 0.32048(16) 0.9846(2) 0.0222(6) Uani 1 1 d . . .
N1 N 0.1730(4) 0.40136(19) 0.7655(3) 0.0209(7) Uani 1 1 d . . .
O2 O -0.1214(4) 0.47662(16) 0.6950(3) 0.0240(7) Uani 1 1 d . . .
C1 C -0.1603(5) 0.2780(2) 0.7364(4) 0.0255(9) Uani 1 1 d . . .
N2 N -0.0243(4) 0.33237(19) 0.7645(3) 0.0216(7) Uani 1 1 d . . .
N3 N -0.3065(4) 0.58466(19) 0.7601(3) 0.0202(7) Uani 1 1 d . . .
C3 C 0.3418(5) 0.3558(2) 1.1806(4) 0.0215(9) Uani 1 1 d . . .
H3A H 0.2762 0.3106 1.1723 0.026 Uiso 1 1 calc R . .
H3B H 0.4692 0.3439 1.2364 0.026 Uiso 1 1 calc R . .
C4 C -0.1200(5) 0.5824(2) 0.8119(4) 0.0217(9) Uani 1 1 d . . .
H4A H -0.0492 0.6060 0.8990 0.026 Uiso 1 1 calc R . .
H4B H -0.1044 0.6122 0.7543 0.026 Uiso 1 1 calc R . .
C5 C -0.4205(6) 0.5918(3) 0.6167(4) 0.0271(10) Uani 1 1 d . . .
H5A H -0.5444 0.5882 0.5833 0.041 Uiso 1 1 calc R . .
H5B H -0.3930 0.5521 0.5791 0.041 Uiso 1 1 calc R . .
H5C H -0.3996 0.6400 0.5925 0.041 Uiso 1 1 calc R . .
C6 C -0.3080(6) 0.3200(3) 0.7270(5) 0.0332(11) Uani 1 1 d . . .
H6A H -0.2623 0.3420 0.8118 0.050 Uiso 1 1 calc R . .
H6B H -0.4039 0.2856 0.7017 0.050 Uiso 1 1 calc R . .
H6C H -0.3527 0.3593 0.6614 0.050 Uiso 1 1 calc R . .
C7 C 0.2542(6) 0.5174(2) 0.7183(4) 0.0295(10) Uani 1 1 d . . .
H7A H 0.1320 0.5259 0.6425 0.044 Uiso 1 1 calc R . .
H7B H 0.3344 0.5412 0.7037 0.044 Uiso 1 1 calc R . .
H7C H 0.2724 0.5387 0.7961 0.044 Uiso 1 1 calc R . .
C8 C -0.0753(6) 0.2230(3) 0.8501(4) 0.0318(10) Uani 1 1 d . . .
H8A H 0.0207 0.1966 0.8570 0.048 Uiso 1 1 calc R . .
H8B H -0.1640 0.1873 0.8348 0.048 Uiso 1 1 calc R . .
H8C H -0.0282 0.2499 0.9314 0.048 Uiso 1 1 calc R . .
C9 C 0.2613(6) 0.4004(3) 0.6166(4) 0.0307(10) Uani 1 1 d . . .
H9A H 0.2789 0.3466 0.6284 0.046 Uiso 1 1 calc R . .
H9B H 0.3454 0.4216 0.6037 0.046 Uiso 1 1 calc R . .
H9C H 0.1408 0.4108 0.5401 0.046 Uiso 1 1 calc R . .
C10 C 0.2907(5) 0.4348(2) 0.7376(4) 0.0235(9) Uani 1 1 d . . .
C11 C -0.0491(5) 0.5055(2) 0.8236(4) 0.0241(9) Uani 1 1 d . . .
H11A H 0.0811 0.5072 0.8763 0.029 Uiso 1 1 calc R . .
H11B H -0.0817 0.4726 0.8682 0.029 Uiso 1 1 calc R . .
C12 C 0.4812(5) 0.4207(3) 0.8558(4) 0.0264(9) Uani 1 1 d . . .
H12A H 0.4992 0.4408 0.9342 0.040 Uiso 1 1 calc R . .
H12B H 0.5620 0.4450 0.8423 0.040 Uiso 1 1 calc R . .
H12C H 0.5042 0.3673 0.8665 0.040 Uiso 1 1 calc R . .
C13 C -0.2358(6) 0.2360(3) 0.6083(4) 0.0323(11) Uani 1 1 d . . .
H13A H -0.2946 0.2711 0.5354 0.048 Uiso 1 1 calc R . .
H13B H -0.3209 0.1990 0.5950 0.048 Uiso 1 1 calc R . .
H13C H -0.1397 0.2113 0.6130 0.048 Uiso 1 1 calc R . .
C14 C 0.2844(5) 0.3806(2) 1.0471(4) 0.0227(9) Uani 1 1 d . . .
H14A H 0.1589 0.3955 0.9933 0.027 Uiso 1 1 calc R . .
H14B H 0.3553 0.4239 1.0561 0.027 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 P2 125.20(11) . . ?
O1 P1 N1 107.13(16) . . ?
O1 P1 N2 107.29(16) . . ?
N1 P1 P2 41.81(11) . . ?
N2 P1 P2 41.80(12) . . ?
N2 P1 N1 80.50(17) . . ?
N1 P2 P1 41.91(12) . . ?
N1 P2 N2 80.42(16) . . ?
O2 P2 P1 126.94(11) . . ?
O2 P2 N1 108.38(16) . . ?
O2 P2 N2 108.65(17) . . ?
N2 P2 P1 41.61(11) . . ?
C14 O1 P1 122.1(2) . . ?
P2 N1 P1 96.29(18) . . ?
C10 N1 P1 126.3(3) . . ?
C10 N1 P2 125.2(3) . . ?
C11 O2 P2 126.5(2) . . ?
N2 C1 C6 108.1(4) . . ?
N2 C1 C8 108.1(3) . . ?
N2 C1 C13 111.7(4) . . ?
C6 C1 C8 109.5(4) . . ?
C6 C1 C13 109.7(4) . . ?
C8 C1 C13 109.8(4) . . ?
P1 N2 P2 96.59(18) . . ?
C1 N2 P1 126.5(3) . . ?
C1 N2 P2 125.3(3) . . ?
C3 N3 C4 111.7(3) 3_567 . ?
C3 N3 C5 110.8(3) 3_567 . ?
C4 N3 C5 110.7(3) . . ?
N3 C3 C14 109.0(3) 3_567 . ?
N3 C4 C11 114.4(3) . . ?
N1 C10 C7 107.9(3) . . ?
N1 C10 C9 111.5(3) . . ?
N1 C10 C12 107.7(3) . . ?
C7 C10 C9 110.3(4) . . ?
C7 C10 C12 110.1(4) . . ?
C9 C10 C12 109.2(4) . . ?
O2 C11 C4 109.7(3) . . ?
O1 C14 C3 109.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 P2 2.5797(14) . ?
P1 O1 1.631(3) . ?
P1 N1 1.733(4) . ?
P1 N2 1.724(3) . ?
P2 N1 1.730(3) . ?
P2 O2 1.624(3) . ?
P2 N2 1.731(4) . ?
O1 C14 1.443(5) . ?
N1 C10 1.482(5) . ?
O2 C11 1.449(5) . ?
C1 N2 1.480(5) . ?
C1 C6 1.528(6) . ?
C1 C8 1.533(6) . ?
C1 C13 1.539(6) . ?
N3 C3 1.462(5) 3_567 ?
N3 C4 1.468(5) . ?
N3 C5 1.477(5) . ?
C3 N3 1.462(5) 3_567 ?
C3 C14 1.517(5) . ?
C4 C11 1.509(6) . ?
C7 C10 1.518(6) . ?
C9 C10 1.529(6) . ?
C10 C12 1.531(5) . ?
