#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/35/4103593.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_4103593
loop_
_publ_author_name
'Zin-Min Tun'
'Matthew J. Panzner'
'Vincenzo Scionti'
'Douglas Medvetz'
'Chrys Wesdemiotis'
'Wiley J. Youngs'
'Claire Tessier'
_publ_section_title
;
 Crown Ether Complexes of HPCl6
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17059
_journal_page_last               17061
_journal_paper_doi               10.1021/ja1064697
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C8 H17 O4, Cl6 P'
_chemical_formula_sum            'C8 H17 Cl6 O4 P'
_chemical_formula_weight         420.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.166(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.638(4)
_cell_length_b                   12.046(6)
_cell_length_c                   17.893(9)
_cell_measurement_reflns_used    1913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.76
_cell_measurement_theta_min      2.75
_cell_volume                     1620.4(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12466
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.30
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.8541
_exptl_absorpt_correction_T_min  0.7840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0414
_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/[σ²(Fo²)+(0.0382P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                2340
_reflns_number_total             3291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1064697_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1620.4(15)
_cod_original_sg_symbol_Hall     -P2yn
_cod_database_code               4103593
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
P1 P 0.62753(10) 0.74780(6) 0.11208(4) 0.01659(19) Uani 1 1 d .
Cl1 Cl 0.52709(10) 0.62378(6) 0.03027(4) 0.0221(2) Uani 1 1 d .
Cl2 Cl 0.89162(10) 0.71609(6) 0.09187(5) 0.0238(2) Uani 1 1 d .
Cl3 Cl 0.59156(11) 0.87225(6) 0.02526(4) 0.0253(2) Uani 1 1 d .
Cl4 Cl 0.36261(10) 0.77914(6) 0.13097(5) 0.0281(2) Uani 1 1 d .
Cl5 Cl 0.65849(11) 0.62298(6) 0.19898(4) 0.0253(2) Uani 1 1 d .
Cl6 Cl 0.73061(10) 0.87078(6) 0.19440(4) 0.0229(2) Uani 1 1 d .
O1 O 0.8246(3) 0.97366(17) 0.82221(12) 0.0247(5) Uani 1 1 d .
O2 O 0.7130(3) 0.74600(16) 0.84736(12) 0.0211(5) Uani 1 1 d .
O3 O 0.9591(3) 0.55979(17) 0.85668(12) 0.0243(5) Uani 1 1 d .
O4 O 1.0235(3) 0.78684(15) 0.90085(12) 0.0187(5) Uani 1 1 d .
C1 C 0.6441(4) 0.9390(3) 0.81416(19) 0.0252(7) Uani 1 1 d .
H1A H 0.5686 0.9876 0.7771 0.030 Uiso 1 1 calc R
H1B H 0.6036 0.9463 0.8635 0.030 Uiso 1 1 calc R
C2 C 0.6235(4) 0.8205(3) 0.78762(18) 0.0267(8) Uani 1 1 d .
H2A H 0.4956 0.8014 0.7751 0.032 Uiso 1 1 calc R
H2B H 0.6759 0.8112 0.7412 0.032 Uiso 1 1 calc R
C3 C 0.6625(4) 0.6294(2) 0.8334(2) 0.0278(8) Uani 1 1 d .
H3A H 0.6617 0.6106 0.7795 0.033 Uiso 1 1 calc R
H3B H 0.5416 0.6167 0.8445 0.033 Uiso 1 1 calc R
C4 C 0.7940(4) 0.5573(3) 0.88362(19) 0.0261(8) Uani 1 1 d .
H4A H 0.8111 0.5849 0.9365 0.031 Uiso 1 1 calc R
H4B H 0.7489 0.4802 0.8829 0.031 Uiso 1 1 calc R
C5 C 1.1103(4) 0.5952(2) 0.90941(19) 0.0256(8) Uani 1 1 d .
H5A H 1.2102 0.5432 0.9083 0.031 Uiso 1 1 calc R
H5B H 1.0821 0.5948 0.9613 0.031 Uiso 1 1 calc R
C6 C 1.1639(4) 0.7097(2) 0.89010(19) 0.0235(7) Uani 1 1 d .
H6A H 1.2768 0.7307 0.9233 0.028 Uiso 1 1 calc R
H6B H 1.1822 0.7122 0.8367 0.028 Uiso 1 1 calc R
C7 C 1.0824(4) 0.9019(2) 0.90351(18) 0.0213(7) Uani 1 1 d .
H7A H 1.1472 0.9165 0.8612 0.026 Uiso 1 1 calc R
H7B H 1.1644 0.9161 0.9519 0.026 Uiso 1 1 calc R
C8 C 0.9256(4) 0.9769(3) 0.89716(17) 0.0241(7) Uani 1 1 d .
H8A H 0.8498 0.9538 0.9339 0.029 Uiso 1 1 calc R
H8B H 0.9663 1.0538 0.9097 0.029 Uiso 1 1 calc R
H' H 0.874(5) 0.771(3) 0.868(2) 0.081(16) Uiso 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'
O O 0.0106 0.0060 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Cl1 P1 Cl6 179.35(5)
Cl1 P1 Cl3 90.46(6)
Cl6 P1 Cl3 89.96(6)
Cl1 P1 Cl4 89.79(5)
Cl6 P1 Cl4 90.71(5)
Cl3 P1 Cl4 89.27(4)
Cl1 P1 Cl2 89.69(5)
Cl6 P1 Cl2 89.81(5)
Cl3 P1 Cl2 90.37(4)
Cl4 P1 Cl2 179.37(5)
Cl1 P1 Cl5 89.24(6)
Cl6 P1 Cl5 90.35(6)
Cl3 P1 Cl5 178.97(5)
Cl4 P1 Cl5 89.74(4)
Cl2 P1 Cl5 90.61(4)
C1 O1 C8 117.2(2)
C3 O2 C2 112.8(2)
C5 O3 C4 116.4(2)
C7 O4 C6 112.4(2)
O1 C1 C2 110.8(2)
O2 C2 C1 109.9(2)
O2 C3 C4 108.9(3)
O3 C4 C3 108.9(3)
O3 C5 C6 110.3(3)
O4 C6 C5 108.6(3)
O4 C7 C8 109.6(2)
O1 C8 C7 110.5(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 Cl1 2.1369(13)
P1 Cl6 2.1389(13)
P1 Cl3 2.1412(13)
P1 Cl4 2.1430(15)
P1 Cl2 2.1454(15)
P1 Cl5 2.1459(13)
O1 C1 1.423(4)
O1 C8 1.425(4)
O2 C3 1.467(4)
O2 C2 1.469(3)
O3 C5 1.422(4)
O3 C4 1.428(4)
O4 C7 1.455(3)
O4 C6 1.457(3)
C1 C2 1.504(4)
C3 C4 1.500(4)
C5 C6 1.496(4)
C7 C8 1.489(4)
