Synthesis and Structure of Cyclic Phosphate, Phosphoramidate, Phosphonates, and Phosphonium Salts. Phosphatrane Formation1
A. Chandrasekaran; Roberta O. Day; Robert R. Holmes; Inorganic Chemistry 39 (2000) 5683–5689; doi:10.1021/ic000467a

data_4321649
_publ_section_title
;
 Synthesis and Structure of Cyclic Phosphate, Phosphoramidate,
 Phosphonates, and Phosphonium Salts. Phosphatrane Formation1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5683
_journal_page_last               5689
_journal_paper_doi               10.1021/ic000467a
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C35 H41 Cl2 I N O4 P'
_chemical_formula_weight         768.46
_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
_cell_angle_alpha                96.27(2)
_cell_angle_beta                 94.06(2)
_cell_angle_gamma                106.00(2)
_cell_formula_units_Z            4
_cell_length_a                   14.174(4)
_cell_length_b                   14.377(4)
_cell_length_c                   19.005(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     3679.8(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4
_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  0.0933
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9010
_diffrn_reflns_theta_max         21.98
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          1.50
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.155
_refine_diff_density_min         -2.509
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.576
_refine_ls_goodness_of_fit_obs   4.095
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         7795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      3.435
_refine_ls_restrained_S_obs      4.095
_refine_ls_R_factor_all          0.2103
_refine_ls_R_factor_obs          0.1558
_refine_ls_shift/esd_max         0.044
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4570
_refine_ls_wR_factor_obs         0.4294
_reflns_number_observed          5786
_reflns_number_total             8973
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000467a_3.cif
_cod_data_source_block           acp34
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321649