Mono-, Di-, and Tricoordinated Phosphorus Attached to a N-N Unit: An Experimental and Theoretical Study
Gerd Fischer; Sebastian Herler; Peter Mayer; Axel Schulz; Alexander Villinger; Jan J. Weigand; Inorganic Chemistry 44 (2005) 1740–1751; doi:10.1021/ic048286m

data_4300785
_publ_contact_author_address
;

Department Chemie und Biochemie

Ludwig-Maximilians Universit\"at

Butenandtstra\&se 5-13 (Haus F)

D-81377 M\"unchen

Bundesrepublik Deutschland

;
_publ_contact_author_email       lex@cup.uni-muenchen.de
_publ_contact_author_fax         +49-89-2180-77492
_publ_contact_author_name        'Axel Schulz'
_publ_section_title
;

Mono-, Di-, and Tricoordinated Phosphorus Attached to a N-N Unit: An

Experimental and Theoretical Study

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1740
_journal_page_last               1751
_journal_paper_doi               10.1021/ic048286m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'P C12 H10 S N2, 3(Si C3 H9)'
_chemical_formula_sum            'C21 H37 N2 P S Si3'
_chemical_formula_weight         464.828
_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               'Mayer, P.'
_audit_block_code                PPhS_NNSIMe3_in251_schulz
_audit_creation_date             28-May-04
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             23-Jun-04
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2525(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.86530(10)
_cell_length_b                   37.6480(4)
_cell_length_c                   16.0046(2)
_cell_measurement_reflns_used    20108
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.134
_cell_volume                     5333.10(11)
_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
;

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_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0773527
_diffrn_orient_matrix_UB_12      -0.0141467
_diffrn_orient_matrix_UB_13      0.0335215
_diffrn_orient_matrix_UB_21      0.0604746
_diffrn_orient_matrix_UB_22      -0.0025494
_diffrn_orient_matrix_UB_23      -0.0505353
_diffrn_orient_matrix_UB_31      0.0558942
_diffrn_orient_matrix_UB_32      0.0223361
_diffrn_orient_matrix_UB_33      0.0154630
_diffrn_radiation_collimation    0.35
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43715
_diffrn_reflns_theta_full        22.97
_diffrn_reflns_theta_max         22.97
_diffrn_reflns_theta_min         3.14
_diffrn_source_current           90.00
_diffrn_source_power             4.050
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           45.00
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.15787(2)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0508P)^2^+1.1752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                4734
_reflns_number_total             7350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048286msi20050120_015141.cif
_cod_data_source_block           in251
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4300785