Conformational and Isomeric Preferences of Six-Membered Inorganic Heterocycles [EtNP(E)(OR)]3 (E = Lone Pair, O, S, or Se): A Synthetic, Spectroscopic, Structural, and Computational Study
Ramaswamy Murugavel; Ganesan Prabusankar; Ashish Sharma; Raghavan B. Sunoj; Ray J. Butcher; Inorganic Chemistry 48 (2009) 2048–2059; doi:10.1021/ic801945q

data_4301563
_publ_contact_author_address
;
Department of Chemistry
Indian Institute of Technology Bombay
Powai
Mumbai
Maharastra
400076
INDIA
;
_publ_contact_author_email       RMV@CHEM.IITB.AC.IN
_publ_contact_author_name        'Ramaswamy Murugavel'
_publ_section_title
;
Conformational and Isomeric Preferences of Six-Membered Inorganic
Heterocycles [EtNP(E)(OR)]3 (E = Lone Pair, O, S, or Se): A Synthetic,
Spectroscopic, Structural, and Computational Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2048
_journal_page_last               2059
_journal_paper_doi               10.1021/ic801945q
_journal_volume                  48
_journal_year                    2009
_chemical_formula_analytical     'C42 H66 N3 O3 P3 '
_chemical_formula_moiety         '[EtNP(OAr)]3'
_chemical_formula_sum            'C42 H66 N3 O3 P3'
_chemical_formula_weight         753.89
_chemical_melting_point          192
_chemical_name_common            cyclotriphosphazane
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           218
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_space_group_name_H-M   'P -4 3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.975(2)
_cell_length_b                   21.975(2)
_cell_length_c                   21.975(2)
_cell_measurement_temperature    200(2)
_cell_volume                     10611.7(17)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    Pluton/Ortep3
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2808
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.9059
_exptl_absorpt_correction_T_min  0.9059
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.944
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic_blocks
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.70
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0574
_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/[\s^2^(Fo^2^)+(0.0623P)^2^+6.5201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                1348
_reflns_number_total             1694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801945q_si_001_2.cif
_cod_data_source_block           mur7
_cod_original_cell_volume        10612.2(18)
_cod_database_code               4301563