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_4301566
_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_sum            'C30 H42 N3 O3 P3 S3'
_chemical_formula_weight         681.76
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.10(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.547(2)
_cell_length_b                   15.144(3)
_cell_length_c                   19.175(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3290.4(12)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_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  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25003
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colouless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.335
_refine_diff_density_min         -1.621
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         6925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1021P)^2^+0.5252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                5068
_reflns_number_total             6925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801945q_si_001_5.cif
_cod_data_source_block           mur53
_cod_original_cell_volume        3290.3(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4301566