Cage Compounds of Heterotrimetallic Mixed Phosphanediide/Silanolate Aggregates with an Alkaline Earth Metal-Centered Phosphorus Octahedron
Matthias Westerhausen; Sabine Weinrich; Gernot Kramer; Holger Piotrowski; Inorganic Chemistry 41 (2002) 7072–7076; doi:10.1021/ic0202413

data_4319055
_publ_author_address
;
Department Chemie
Ludwig-Maximilians-Universitaet
Butenandtstr. 9 (House D)
D-81377 Muenchen, Germany
;
_publ_contact_author
;
    Matthias Westerhausen
    Department Chemie
    Ludwig-Maximilians-Universitaet Muenchen
    Butenandtstr. 9 (House D)
    D-81377 Muenchen
    Germany
;
_publ_contact_author_email       maw@cup.uni-muenchen.de
_publ_contact_author_fax         +49(0)89/2180-7867
_publ_contact_author_phone       +49(0)89/2180-7481
_publ_section_title
;
 Cage Compounds of Heterotrimetallic Mixed Phosphanediide/Silanolate
 Aggregates with an Alkaline Earth Metal-Centered Phosphorus Octahedron
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7072
_journal_page_last               7076
_journal_paper_doi               10.1021/ic0202413
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source
;
crystals provided by S. Weinrich
;
_chemical_formula_moiety
'Sr K6 Li6 6(P Si 3(C3 H7)) 2(O Si 3(C H3)), 2(C7 H8)''
_chemical_formula_sum            'C74 H160 K6 Li6 O2 P6 Si8 Sr'
_chemical_formula_weight         1856.44
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.5700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.8124(3)
_cell_length_b                   16.0122(3)
_cell_length_c                   18.5926(4)
_cell_measurement_reflns_used    37646
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      3.134
_cell_volume                     5302.64(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
'SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_collimation    0.25
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44852
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         3.15
_diffrn_source_current           75.00
_diffrn_source_power             4.125
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  0.9782
_exptl_absorpt_correction_T_min  0.9200
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.16272(4)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         9608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0336P)^2^+2.8846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                6688
_reflns_number_total             9608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0202413_1.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '_publ_author_adress' replaced with '_publ_author_address'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
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_cod_database_code               4319055
_kl_diffrn_measurement_scan_angle phi/omega-scan
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_kl_diffrn_measurement_scan_time_per_degree 600
_kl_diffrn_measurement_detector_distance 30