Preparations of Metal Trichalcogenophosphonates from Organophosphonate Esters
Robert P. Davies; Laura Patel; Andrew J. P. White; Inorganic Chemistry 51 (2012) 11594–11601; doi:10.1021/ic301504p

data_4330856
_publ_section_title
;
 Preparations of Metal Trichalcogenophosphonates from Organophosphonate
 Esters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11594
_journal_page_last               11601
_journal_paper_doi               10.1021/ic301504p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C34 H62 Li4 N4 O2 P2 S6, C4 H8 O'
_chemical_formula_sum            'C38 H70 Li4 N4 O3 P2 S6'
_chemical_formula_weight         913.04
_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                94.743(4)
_cell_angle_beta                 91.093(4)
_cell_angle_gamma                110.391(4)
_cell_formula_units_Z            1
_cell_length_a                   8.8544(4)
_cell_length_b                   10.7325(5)
_cell_length_c                   14.0520(6)
_cell_measurement_reflns_used    9376
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.4571
_cell_measurement_theta_min      2.5739
_cell_volume                     1245.76(10)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17413
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         32.48
_diffrn_reflns_theta_min         2.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       blocks
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         8173
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                6262
_reflns_number_total             8173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301504p_si_003_1.cif
_cod_data_source_block           1
_cod_database_code               4330856