Synthesis and structure of a tris imido phosphonate anion; the missing link in imido analogues of phosphorus oxoanions
Burke, Lisa T.; Hevia-Freire, Eva; Holland, Rebecca; Jeffery, John C.; Leedham, Angela P.; Russell, Christopher A.; Zagorski, Anette; Steiner, Alexander; Chemical Communications  (2000) 1769–; doi:10.1039/b004192k

data_7111018
_publ_section_title
;
 Synthesis and structure of a tris imido phosphonate anion; the missing
 link in imido analogues of phosphorus oxoanions
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1769
_journal_paper_doi               10.1039/b004192k
_journal_year                    2000
_chemical_formula_sum            'C21 H22 Li2 N3 O3 P'
_chemical_formula_weight         409.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.026(5)
_cell_length_b                   11.410(2)
_cell_length_c                   22.560(5)
_cell_measurement_temperature    173(2)
_cell_volume                     4125.2(17)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method
'\w rotation with narrow frames (0.3 degrees)'
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24588
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.015
_refine_ls_goodness_of_fit_obs   1.065
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.065
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_obs          0.0402
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+1.0795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1042
_refine_ls_wR_factor_obs         0.0920
_reflns_number_observed          3407
_reflns_number_total             4710
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004192ksup1.cif
_cod_data_source_block           cad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+1.0795P] 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^)+(0.0499P)^2^+1.0795P] 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        4125.4(17)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7111018