Unexpected formation of ansa isomers enabled by phosphazene ring flexibility in the reactions of cyclotetraphosphazene with 1,2-ethanediol.
Palabıyık, Duygu; Mutlu Balcı, Ceylan; Allen, Christopher W.; Beşli, Serap; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6673–6681; doi:10.1039/d1dt00386k

data_7707090
_publ_section_title
;
 Unexpected formation of ansa isomers enabled by phosphazene ring
 flexibility in the reactions of cyclotetraphosphazene with
 1,2-ethanediol.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6673
_journal_page_last               6681
_journal_paper_doi               10.1039/d1dt00386k
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration none
_chemical_formula_moiety         'C4 H8 Cl4 N4 O4 P4'
_chemical_formula_sum            'C4 H8 Cl4 N4 O4 P4'
_chemical_formula_weight         441.82
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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_creation_date             2020-12-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-13 deposited with the CCDC.	2021-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                69.92(2)
_cell_angle_beta                 70.932(14)
_cell_angle_gamma                72.958(15)
_cell_formula_units_Z            1
_cell_length_a                   5.9782(14)
_cell_length_b                   8.5423(19)
_cell_length_c                   8.728(2)
_cell_measurement_reflns_used    2362
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      2.57
_cell_volume                     387.35(16)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.1152
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5921
_diffrn_reflns_point_group_measured_fraction_full 0.845
_diffrn_reflns_point_group_measured_fraction_max 0.759
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.789
_diffrn_reflns_theta_min         2.567
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  0.7411
_exptl_absorpt_correction_T_min  0.5078
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1624 before and 0.0848 after correction.
The Ratio of minimum to maximum transmission is 0.6852.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       Plate
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.086
_refine_diff_density_max         2.348
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.283
_refine_ls_abs_structure_details
;
 Flack x determined using 631 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.336
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3057
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.353
_refine_ls_R_factor_all          0.1660
_refine_ls_R_factor_gt           0.1416
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3547
_refine_ls_wR_factor_ref         0.3687
_reflns_Friedel_coverage         0.599
_reflns_Friedel_fraction_full    0.700
_reflns_Friedel_fraction_max     0.569
_reflns_number_gt                2167
_reflns_number_total             3057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00386k2.cif
_cod_data_source_block           19gtu125_319_dp_teg_1
_cod_depositor_comments
'Adding full bibliography for 7707090--7707092.cif.'
_cod_original_cell_volume        387.37(18)
_cod_database_code               7707090
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.690
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
N3 \\sim P4: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.02
within 2A
O4 \\sim C4: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.02
within 2A
Cl3 \\sim P4: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.02 within 2A
Cl4 \\sim P4: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.02 within 2A
C3 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C1(H1A,H1B), C3(H3A,H3B)
;
_shelx_res_checksum              9113
_shelx_hkl_checksum              38607
_olex2_submission_special_instructions 'No special instructions were received'