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_4301567
_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            'C42 H66 N3 O3 P3 Se3'
_chemical_formula_weight         990.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.452(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.652(3)
_cell_length_b                   9.8500(18)
_cell_length_c                   25.85(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4741(9)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            8623
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.09
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.467
_exptl_absorpt_correction_T_max  0.4757
_exptl_absorpt_correction_T_min  0.3829
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .33
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+2.1451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                5837
_reflns_number_total             8348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801945q_si_001_6.cif
_cod_data_source_block           rm115c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4741(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301567