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#$Date: 2016-03-23 16:41:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179389 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/86/4328610.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4328610
loop_
_publ_author_name
'Michael H. Holthausen'
'Kai-Oliver Feldmann'
'Stephen Schulz'
'Alexander Hepp'
'Jan J. Weigand'
_publ_section_title
;
 Formation of Cationic [RP5Cl]+-Cages via Insertion of [RPCl]+-Cations
 into a P-P Bond of the P4 Tetrahedron
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3374
_journal_page_last               3387
_journal_paper_doi               10.1021/ic2013304
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C6 H5 Cl P5, Cl4 Ga '
_chemical_formula_sum            'C6 H5 Cl5 Ga P5'
_chemical_formula_weight         478.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.3070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4378(5)
_cell_length_b                   15.2665(9)
_cell_length_c                   12.3411(7)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     1588.44(16)
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(1)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17396
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    3.050
_exptl_absorpt_correction_T_max  0.9415
_exptl_absorpt_correction_T_min  0.7709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax =  0.781934 

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0173P)²+0.4913P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0423
_reflns_number_gt                3803
_reflns_number_total             4266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2013304_si_006.cif
_cod_data_source_block           sad
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328610
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.94083(17) 0.68095(9) 0.54792(11) 0.0168(3) Uani 1 1 d .
C2 C 0.80115(18) 0.65441(10) 0.59446(12) 0.0221(3) Uani 1 1 d .
H2 H 0.7087 0.6899 0.5880 0.027 Uiso 1 1 calc R
C3 C 0.7983(2) 0.57560(11) 0.65043(13) 0.0277(3) Uani 1 1 d .
H3 H 0.7039 0.5573 0.6832 0.033 Uiso 1 1 calc R
C4 C 0.9327(2) 0.52366(10) 0.65854(13) 0.0273(3) Uani 1 1 d .
H4 H 0.9296 0.4696 0.6965 0.033 Uiso 1 1 calc R
C5 C 1.0718(2) 0.54976(10) 0.61187(13) 0.0261(3) Uani 1 1 d .
H5 H 1.1635 0.5137 0.6179 0.031 Uiso 1 1 calc R
C6 C 1.07705(18) 0.62822(10) 0.55658(12) 0.0211(3) Uani 1 1 d .
H6 H 1.1722 0.6464 0.5246 0.025 Uiso 1 1 calc R
P1 P 0.95712(4) 0.78455(2) 0.48216(3) 0.01593(7) Uani 1 1 d .
P2 P 1.09762(5) 0.78989(3) 0.33967(3) 0.02217(9) Uani 1 1 d .
P3 P 1.11303(5) 0.87810(3) 0.56402(3) 0.02107(8) Uani 1 1 d .
P4 P 1.15691(5) 0.92662(3) 0.39574(4) 0.02727(9) Uani 1 1 d .
P5 P 1.29764(5) 0.81853(3) 0.46098(3) 0.02118(8) Uani 1 1 d .
Cl1 Cl 0.73707(4) 0.83141(3) 0.45586(3) 0.02556(8) Uani 1 1 d .
Cl2 Cl 0.19591(4) 0.15299(2) 0.24404(3) 0.02215(8) Uani 1 1 d .
Cl3 Cl 0.53090(4) 0.04305(2) 0.35891(3) 0.02411(8) Uani 1 1 d .
Cl4 Cl 0.52733(5) 0.10634(3) 0.08223(3) 0.02815(9) Uani 1 1 d .
Cl5 Cl 0.55636(4) 0.27019(2) 0.28766(3) 0.02192(8) Uani 1 1 d .
Ga1 Ga 0.454880(18) 0.143092(10) 0.241726(13) 0.01669(4) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C2 C1 C6 120.39(14)
C2 C1 P1 121.82(11)
C6 C1 P1 117.70(11)
C3 C2 C1 119.32(15)
C3 C2 H2 120.3
C1 C2 H2 120.3
C4 C3 C2 120.12(15)
C4 C3 H3 119.9
C2 C3 H3 119.9
C3 C4 C5 120.68(15)
C3 C4 H4 119.7
C5 C4 H4 119.7
C6 C5 C4 119.94(15)
C6 C5 H5 120.0
C4 C5 H5 120.0
C5 C6 C1 119.54(14)
C5 C6 H6 120.2
C1 C6 H6 120.2
C1 P1 Cl1 107.58(5)
C1 P1 P2 117.26(5)
Cl1 P1 P2 112.94(2)
C1 P1 P3 115.39(5)
Cl1 P1 P3 112.45(2)
P2 P1 P3 90.68(2)
P1 P2 P4 84.68(2)
P1 P2 P5 83.541(19)
P4 P2 P5 57.597(18)
P1 P3 P5 83.73(2)
P1 P3 P4 84.60(2)
P5 P3 P4 57.737(19)
P5 P4 P2 61.298(19)
P5 P4 P3 60.974(18)
P2 P4 P3 86.31(2)
P4 P5 P3 61.29(2)
P4 P5 P2 61.105(19)
P3 P5 P2 86.37(2)
Cl4 Ga1 Cl3 109.630(17)
Cl4 Ga1 Cl5 110.166(16)
Cl3 Ga1 Cl5 110.350(16)
Cl4 Ga1 Cl2 110.417(16)
Cl3 Ga1 Cl2 107.836(16)
Cl5 Ga1 Cl2 108.403(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.392(2)
C1 C6 1.404(2)
C1 P1 1.7855(15)
C2 C3 1.388(2)
C2 H2 0.9500
C3 C4 1.384(2)
C3 H3 0.9500
C4 C5 1.387(2)
C4 H4 0.9500
C5 C6 1.380(2)
C5 H5 0.9500
C6 H6 0.9500
P1 Cl1 2.0040(5)
P1 P2 2.1615(5)
P1 P3 2.1644(5)
P2 P4 2.2491(6)
P2 P5 2.2533(5)
P3 P5 2.2428(6)
P3 P4 2.2496(6)
P4 P5 2.1690(6)
Cl2 Ga1 2.1917(4)
Cl3 Ga1 2.1819(4)
Cl4 Ga1 2.1587(4)
Cl5 Ga1 2.1864(4)
