Apical versus Equatorial Disposition of Substituents in Tetraoxyphosphoranes Bearing a 1,3,2-Dioxaphosphocin Ring: Implications on Apicophilicity in Trigonal Bipyramidal Phosphorus
Praveen Kommana; Sudha Kumaraswamy; J. J. Vittal; K. C. Kumara Swamy; Inorganic Chemistry 41 (2002) 2356–2363; doi:10.1021/ic010935w

data_4317920
_publ_section_title
;
 Apical versus Equatorial Disposition of Substituents in
 Tetraoxyphosphoranes Bearing a 1,3,2-Dioxaphosphocin Ring: Implications
 on Apicophilicity in Trigonal Bipyramidal Phosphorus
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2356
_journal_page_last               2363
_journal_paper_doi               10.1021/ic010935w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C33.5 H38 Cl4 N O4 P S'
_chemical_formula_weight         723.48
_chemical_name_systematic
;

  ?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.986(18)
_cell_angle_beta                 78.85(4)
_cell_angle_gamma                73.25(3)
_cell_formula_units_Z            2
_cell_length_a                   9.563(2)
_cell_length_b                   12.993(2)
_cell_length_c                   15.994(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1806.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6348
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        5%
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+4.9768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2216
_refine_ls_wR_factor_ref         0.2582
_reflns_number_gt                3248
_reflns_number_total             6348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010935w_5.cif
_cod_data_source_block           compd5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+4.9768P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+4.9768P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1806.7(6)
_cod_original_formula_sum        'C33.50 H38 Cl4 N O4 P S'
_cod_database_code               4317920