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_4321650
_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            'C30.5 H36.5 Cl2 I3 N O3.25 P'
_chemical_formula_weight         951.68
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.44(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.515(5)
_cell_length_b                   20.625(6)
_cell_length_c                   24.177(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     7225(4)
_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  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8911
_diffrn_reflns_theta_max         22.02
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    2.819
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_F_000             3684
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.60
_refine_diff_density_max         2.227
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.211
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         7102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.385
_refine_ls_restrained_S_obs      1.211
_refine_ls_R_factor_all          0.1758
_refine_ls_R_factor_obs          0.0911
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1655P)^2^+80.5575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4028
_refine_ls_wR_factor_obs         0.2585
_reflns_number_observed          4719
_reflns_number_total             8832
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000467a_4.cif
_cod_data_source_block           acp36
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1655P)^2^+80.5575P] 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^)+(0.1655P)^2^+80.5575P] 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        7224.9(40)
_cod_original_formula_sum        'C30.50 H36.50 Cl2 I3 N O3.25 P'
_cod_database_code               4321650