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_4319056
_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
;
crystal provided by S. Weinrich
;
_chemical_formula_moiety
'Ba, K6, Li6, 6(P Si C9 H21), 2(O Si C3 H9), 2(C7 H8)'
_chemical_formula_sum            'C74 H160 Ba K6 Li6 O2 P6 Si8'
_chemical_formula_weight         1906.150
_chemical_name_common            Ba-K-PSi(iPr)3-Li-OSiMe3
_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
_audit_author_name               'Piotrowski, H.'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.904(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.6791(12)
_cell_length_b                   16.0693(8)
_cell_length_c                   17.7442(11)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      1.7
_cell_volume                     5325.4(5)
_computing_cell_refinement       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_collection       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_reduction        'Stoe IPDS software (Darmstadt, Germany)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'image-plate area detector'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37148
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         1.67
_diffrn_source_current           50_mA
_diffrn_source_power             2.75_kW
_diffrn_source_type              'Spellman DF4 Series'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.9143
_exptl_absorpt_correction_T_min  0.8416
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.18875(11)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         10302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                7667
_reflns_number_total             10302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0202413_2.cif
_cod_data_source_block           Compound2
_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 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4319056
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 180.0
_kl_diffrn_detector_area_phi_incr 1.0
_kl_diffrn_detector_area_expos_time 6.00_min
_kl_diffrn_detector_area_plate_dist 70.0_mm
_kl_diffrn_detector_area_eff_mos_spread 0.006
_kl_diffrn_detector_area_profile_funct dynamic
_kl_diffrn_detector_area_profile_min 9
_kl_diffrn_detector_area_profile_max 19