#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:59:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180117 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/15/7101515.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_7101515
loop_
_publ_author_name
'Oliver C. Presly'
'Michael Green'
'John C. Jeffery'
'Eva Leiner'
'Martin Murray'
'Christopher A. Russell'
'Manfred Scheer'
'Ulf Vogel'
_publ_section_title
;
The surprising and stereoselective formation of P2C10
cages by the reduction of Cp*PCl2
;
_journal_issue                   43
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b611484a
_journal_year                    2006
_chemical_formula_sum            'C20 H30 Cl3 Ga P2'
_chemical_formula_weight         508.45
_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                 101.54(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.861(3)
_cell_length_b                   10.475(2)
_cell_length_c                   17.101(3)
_cell_measurement_reflns_used    1459
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.29
_cell_volume                     2257.2(8)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software'
_computing_molecular_graphics    SIEMENS-XP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'STOE IPDS'
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12872
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    1.719
_exptl_absorpt_correction_T_max  0.8151
_exptl_absorpt_correction_T_min  0.5653
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'program faceit'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0294
_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/[σ²(Fo²)+(0.0546P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                3671
_reflns_number_total             4374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b611484a.txt
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7101515
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
Ga Ga 0.271075(17) 0.08980(2) 0.137668(13) 0.02317(8) Uani 1 1 d .
Cl1 Cl 0.30541(4) 0.28016(5) 0.18647(4) 0.03432(14) Uani 1 1 d .
Cl2 Cl 0.13478(4) 0.09643(6) 0.03902(3) 0.03375(14) Uani 1 1 d .
Cl3 Cl 0.40495(5) 0.00167(7) 0.09879(4) 0.04372(16) Uani 1 1 d .
P1 P 0.22694(4) -0.03308(5) 0.24433(3) 0.01921(12) Uani 1 1 d .
P2 P 0.13065(4) 0.04334(5) 0.32531(3) 0.02219(13) Uani 1 1 d .
C1 C 0.12141(15) -0.1625(2) 0.23127(12) 0.0222(4) Uani 1 1 d .
C2 C 0.16994(16) -0.2928(2) 0.24099(12) 0.0238(4) Uani 1 1 d .
C3 C 0.20151(16) -0.32219(19) 0.31879(12) 0.0239(4) Uani 1 1 d .
C4 C 0.18082(16) -0.21245(19) 0.37288(12) 0.0213(4) Uani 1 1 d .
C5 C 0.09370(15) -0.1330(2) 0.31448(12) 0.0221(4) Uani 1 1 d .
C6 C 0.28064(16) -0.1213(2) 0.39764(12) 0.0217(4) Uani 1 1 d .
C7 C 0.33916(15) -0.08653(19) 0.32777(12) 0.0213(4) Uani 1 1 d .
C8 C 0.39145(16) 0.0405(2) 0.35524(12) 0.0241(4) Uani 1 1 d .
C9 C 0.33605(17) 0.0999(2) 0.40279(13) 0.0248(4) Uani 1 1 d .
C10 C 0.24399(16) 0.0171(2) 0.41444(12) 0.0230(4) Uani 1 1 d .
C11 C 0.03408(17) -0.1383(2) 0.15766(14) 0.0315(5) Uani 1 1 d .
H11A H 0.0074 -0.0509 0.1594 0.047 Uiso 1 1 calc R
H11B H -0.0241 -0.1989 0.1572 0.047 Uiso 1 1 calc R
H11C H 0.0631 -0.1496 0.1093 0.047 Uiso 1 1 calc R
C12 C 0.1864(2) -0.3668(2) 0.16980(14) 0.0355(5) Uani 1 1 d .
H12A H 0.2324 -0.3183 0.1413 0.053 Uiso 1 1 calc R
H12B H 0.1178 -0.3820 0.1342 0.053 Uiso 1 1 calc R
H12C H 0.2199 -0.4488 0.1872 0.053 Uiso 1 1 calc R
C13 C 0.2540(2) -0.4444(2) 0.35167(15) 0.0344(5) Uani 1 1 d .
H13A H 0.2149 -0.4812 0.3899 0.052 Uiso 1 1 calc R
H13B H 0.3272 -0.4268 0.3786 0.052 Uiso 1 1 calc R
H13C H 0.2540 -0.5048 0.3079 0.052 Uiso 1 1 calc R
C14 C 0.14182(19) -0.2655(2) 0.44607(13) 0.0301(5) Uani 1 1 d .
H14A H 0.1210 -0.1946 0.4770 0.045 Uiso 1 1 calc R
H14B H 0.1990 -0.3142 0.4795 0.045 Uiso 1 1 calc R
H14C H 0.0806 -0.3215 0.4282 0.045 Uiso 1 1 calc R
C15 C -0.02092(16) -0.1629(2) 0.31897(14) 0.0300(5) Uani 1 1 d .
H15A H -0.0328 -0.1421 0.3724 0.045 Uiso 1 1 calc R
H15B H -0.0349 -0.2539 0.3083 0.045 Uiso 1 1 calc R
H15C H -0.0688 -0.1121 0.2791 0.045 Uiso 1 1 calc R
C16 C 0.36346(18) -0.1732(2) 0.46858(13) 0.0307(5) Uani 1 1 d .
H16A H 0.3878 -0.2574 0.4549 0.046 Uiso 1 1 calc R
H16B H 0.3311 -0.1806 0.5156 0.046 Uiso 1 1 calc R
H16C H 0.4240 -0.1146 0.4802 0.046 Uiso 1 1 calc R
C17 C 0.2034(2) 0.0432(2) 0.49124(14) 0.0353(5) Uani 1 1 d .
H17A H 0.2564 0.0146 0.5373 0.053 Uiso 1 1 calc R
H17B H 0.1369 -0.0033 0.4897 0.053 Uiso 1 1 calc R
H17C H 0.1910 0.1349 0.4959 0.053 Uiso 1 1 calc R
C18 C 0.3530(2) 0.2313(2) 0.43772(15) 0.0364(5) Uani 1 1 d .
H18A H 0.3725 0.2252 0.4960 0.055 Uiso 1 1 calc R
H18B H 0.2874 0.2808 0.4227 0.055 Uiso 1 1 calc R
H18C H 0.4101 0.2736 0.4173 0.055 Uiso 1 1 calc R
C19 C 0.48865(17) 0.0863(2) 0.32784(15) 0.0336(5) Uani 1 1 d .
H19A H 0.4766 0.0826 0.2695 0.050 Uiso 1 1 calc R
H19B H 0.5490 0.0318 0.3506 0.050 Uiso 1 1 calc R
H19C H 0.5039 0.1746 0.3455 0.050 Uiso 1 1 calc R
C20 C 0.41275(17) -0.1846(2) 0.30135(14) 0.0303(5) Uani 1 1 d .
H20A H 0.3723 -0.2616 0.2823 0.046 Uiso 1 1 calc R
H20B H 0.4697 -0.2064 0.3466 0.046 Uiso 1 1 calc R
H20C H 0.4436 -0.1487 0.2582 0.046 Uiso 1 1 calc R
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
Cl3 Ga Cl1 113.27(3)
Cl3 Ga Cl2 109.94(3)
Cl1 Ga Cl2 109.79(2)
Cl3 Ga P1 109.17(3)
Cl1 Ga P1 105.19(3)
Cl2 Ga P1 109.33(3)
C1 P1 C7 107.20(9)
C1 P1 P2 81.59(7)
C7 P1 P2 94.22(7)
C1 P1 Ga 124.56(7)
C7 P1 Ga 118.10(7)
P2 P1 Ga 122.48(3)
C10 P2 C5 94.22(9)
C10 P2 P1 90.81(7)
C5 P2 P1 75.26(7)
C2 C1 C11 117.59(18)
C2 C1 C5 104.15(16)
C11 C1 C5 116.87(17)
C2 C1 P1 111.44(13)
C11 C1 P1 111.60(14)
C5 C1 P1 92.28(12)
C3 C2 C12 128.5(2)
C3 C2 C1 110.79(18)
C12 C2 C1 120.47(19)
C2 C3 C13 126.1(2)
C2 C3 C4 111.74(18)
C13 C3 C4 122.18(19)
C3 C4 C14 110.10(17)
C3 C4 C5 101.55(15)
C14 C4 C5 113.45(17)
C3 C4 C6 112.56(16)
C14 C4 C6 112.15(16)
C5 C4 C6 106.56(16)
C15 C5 C1 113.81(17)
C15 C5 C4 115.52(18)
C1 C5 C4 102.08(15)
C15 C5 P2 114.77(15)
C1 C5 P2 100.45(13)
C4 C5 P2 108.49(13)
C16 C6 C10 111.53(17)
C16 C6 C7 108.53(16)
C10 C6 C7 97.60(16)
C16 C6 C4 113.03(17)
C10 C6 C4 110.37(16)
C7 C6 C4 114.81(16)
C8 C7 C20 114.71(17)
C8 C7 C6 102.49(16)
C20 C7 C6 119.19(17)
C8 C7 P1 101.34(13)
C20 C7 P1 113.53(14)
C6 C7 P1 103.36(12)
C9 C8 C19 128.3(2)
C9 C8 C7 109.76(19)
C19 C8 C7 121.9(2)
C8 C9 C18 128.1(2)
C8 C9 C10 109.85(18)
C18 C9 C10 121.9(2)
C9 C10 C17 114.86(18)
C9 C10 C6 103.54(17)
C17 C10 C6 119.26(18)
C9 C10 P2 107.77(14)
C17 C10 P2 108.82(15)
C6 C10 P2 101.34(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ga Cl3 2.1717(8)
Ga Cl1 2.1725(7)
Ga Cl2 2.1773(9)
Ga P1 2.3917(7)
P1 C1 1.899(2)
P1 C7 1.900(2)
P1 P2 2.1858(9)
P2 C10 1.907(2)
P2 C5 1.907(2)
C1 C2 1.496(3)
C1 C11 1.531(3)
C1 C5 1.565(3)
C2 C3 1.347(3)
C2 C12 1.494(3)
C3 C13 1.502(3)
C3 C4 1.532(3)
C4 C14 1.542(3)
C4 C5 1.580(3)
C4 C6 1.588(3)
C5 C15 1.524(3)
C6 C16 1.545(3)
C6 C10 1.568(3)
C6 C7 1.577(3)
C7 C8 1.522(3)
C7 C20 1.525(3)
C8 C9 1.337(3)
C8 C19 1.499(3)
C9 C18 1.498(3)
C9 C10 1.513(3)
C10 C17 1.532(3)
