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_4330860
_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         'C18 H46 Mg2 N4 P2 Se6, 2(C H2 Cl2)'
_chemical_formula_sum            'C20 H50 Cl4 Mg2 N4 P2 Se6'
_chemical_formula_weight         1072.76
_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                68.813(4)
_cell_angle_beta                 76.831(3)
_cell_angle_gamma                86.348(3)
_cell_formula_units_Z            1
_cell_length_a                   10.1998(3)
_cell_length_b                   10.2810(4)
_cell_length_c                   10.4612(4)
_cell_measurement_reflns_used    5558
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.5404
_cell_measurement_theta_min      2.8748
_cell_volume                     995.74(7)
_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 15.9825
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.894
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11086
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         31.61
_diffrn_reflns_theta_min         2.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.911
_exptl_absorpt_correction_T_max  0.594
_exptl_absorpt_correction_T_min  0.491
_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    1.789
_exptl_crystal_description       tablets
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         5969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0488
_reflns_number_gt                4127
_reflns_number_total             5969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301504p_si_003_5.cif
_cod_data_source_block           5
_cod_original_cell_volume        995.75(6)
_cod_database_code               4330860