Characterization of Stereoisomers of Spirophosphoranes Bearing an Eight-Membered Ring: Implications on Apicophilicity in Trigonal Bipyramidal Phosphorus
Sudha Kumaraswamy; C. Muthiah; K. C. Kumara Swamy; Journal of the American Chemical Society 122 (2000) 964–965; doi:10.1021/ja992304v

data_4115906
_publ_section_title
;
 Characterization of Stereoisomers of Spirophosphoranes Bearing an
 Eight-Membered Ring: Implications on Apicophilicity in Trigonal
 Bipyramidal Phosphorus
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              964
_journal_page_last               965
_journal_paper_doi               10.1021/ja992304v
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C38.5 H38 Cl5 O4 P S'
_chemical_formula_weight         804.97
_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                82.49(3)
_cell_angle_beta                 79.47(3)
_cell_angle_gamma                85.56(5)
_cell_formula_units_Z            2
_cell_length_a                   11.656(6)
_cell_length_b                   12.354(9)
_cell_length_c                   13.738(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1925.3(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    0.0302
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5805
_diffrn_reflns_theta_full        23.67
_diffrn_reflns_theta_max         23.67
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.512
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         3608
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1592P)^2^+0.2979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.2435
_reflns_number_gt                3608
_reflns_number_total             5805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992304v_4.cif
_cod_data_source_block           compound7(Kumara_Swamy)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'triclinc' was replaced with
'triclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1592P)^2^+0.2979P] 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^)+(0.1592P)^2^+0.2979P] 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        1925.4(18)
_cod_original_formula_sum        'C38.50 H38 Cl5 O4 P S'
_cod_database_code               4115906