Facile Synthesis of Bis(dichalcogenophosphinate)s and a Remarkable [Li8(OH)6]2+ Polyhedron
Robert P. Davies; M. Giovanna Martinelli; Laura Patel; Andrew J. P. White; Inorganic Chemistry 49 (2010) 4626–4631; doi:10.1021/ic100272y

data_4315509
_publ_section_title
;
 Facile Synthesis of Bis(dichalcogenophosphinate)s and a Remarkable
 [Li8(OH)6]2+ Polyhedron
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4626
_journal_page_last               4631
_journal_paper_doi               10.1021/ic100272y
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'C38 H62 Li2 O6 P2 Se4, C30 H46 Li2 O4 P2 Se4'
_chemical_formula_sum            'C68 H108 Li4 O10 P4 Se8'
_chemical_formula_weight         1868.86
_chemical_name_common            3
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.38(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.969(5)
_cell_length_b                   13.379(3)
_cell_length_c                   18.139(7)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.53
_cell_measurement_theta_min      5.22
_cell_volume                     4117(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      183(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5544
_diffrn_reflns_theta_full        22.51
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        4.93
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.678
_exptl_absorpt_correction_T_max  0.1834
_exptl_absorpt_correction_T_min  0.1587
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Bruker XPREP'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5334
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                3543
_reflns_number_total             5334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100272y_si_001_2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315509