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_4300783
_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         'C15 H32 Cl N2 P Si3'
_chemical_formula_sum            'C15 H32 Cl N2 P Si3'
_chemical_formula_weight         391.111
_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                P_Cl_Ph_N2_SiMe3_h113_schulz
_audit_creation_date             29-Aug-03
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_audit_update_record             23-Jun-04
_cell_angle_alpha                90.00
_cell_angle_beta                 110.908(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5811(12)
_cell_length_b                   9.2489(8)
_cell_length_c                   16.2147(11)
_cell_measurement_reflns_used    3882
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.3
_cell_volume                     2182.8(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'image-plate area detector'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_diffrn_orient_matrix_type
;first index: i in a~i~^*^, second: diffractometer xyz

 e.g. UB_21,UB_22,UB_23 are the xyz components of b^*^

;
_diffrn_orient_matrix_UB_11      0.060043
_diffrn_orient_matrix_UB_12      0.007224
_diffrn_orient_matrix_UB_13      -0.032603
_diffrn_orient_matrix_UB_21      -0.050974
_diffrn_orient_matrix_UB_22      0.045493
_diffrn_orient_matrix_UB_23      -0.083798
_diffrn_orient_matrix_UB_31      0.027878
_diffrn_orient_matrix_UB_32      0.058048
_diffrn_orient_matrix_UB_33      0.014554
_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  0.0943
_diffrn_reflns_av_sigmaI/netI    0.1327
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10197
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.26
_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    0.412
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.19015(16)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.777
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.777
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                1573
_reflns_number_total             2838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048286msi20050120_015024.cif
_cod_data_source_block           h113
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'momoclinic' was replaced with
'monoclinic' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4300783