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_4321647
_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            'C18 H20 N O3 P'
_chemical_formula_weight         329.32
_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                86.36(2)
_cell_angle_beta                 89.46(2)
_cell_angle_gamma                85.86(2)
_cell_formula_units_Z            4
_cell_length_a                   9.837(2)
_cell_length_b                   11.168(4)
_cell_length_c                   15.462(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     1690.8(8)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4140
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_F_000             696
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_obs          0.0377
_refine_ls_shift/esd_max         -0.021
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.6263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1262
_refine_ls_wR_factor_obs         0.0989
_reflns_number_observed          2754
_reflns_number_total             4140
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000467a_1.cif
_cod_data_source_block           acp30
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.6263P] 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^)+(0.0601P)^2^+0.6263P] 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               4321647