#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:41:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179342 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/39/4323985.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_4323985
loop_
_publ_author_name
'Linfeng Chen'
'F. Albert Cotton'
_publ_section_title
;
 Synthesis, Structure, and Reactivity of [Zr6Cl18H5]2-, the First
 Paramagnetic Species of Its Class
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7364
_journal_page_last               7369
_journal_paper_doi               10.1021/ic960454q
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source
'reaction of (Ph4P)3[Zr6Cl18H5] with excess of TiCl4'
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         '2(C24 H20 P),Zr2 Ti2 Cl16'
_chemical_formula_structural     (Ph4P)2[Zr2Ti2Cl16]
_chemical_formula_sum            'C48 H40 Cl16 P2 Ti2 Zr2'
_chemical_formula_weight         1524.18
_chemical_name_systematic
; 
 bis(tetraphenylphosphonium)[octachloro-dizirconium-dititanium] 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                106.07(1)
_cell_angle_beta                 114.77(1)
_cell_angle_gamma                88.50(1)
_cell_formula_units_Z            1
_cell_length_a                   11.375(3)
_cell_length_b                   13.357(3)
_cell_length_c                   11.336(3)
_cell_measurement_reflns_used    211
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.0
_cell_volume                     1494.8(7)
_computing_cell_refinement       Madnes
_computing_data_collection       'MicroVax 3900'
_computing_data_reduction        absurd
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Enraf-Nonius FAST'
_diffrn_measurement_method       'frame data from omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8878
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         2.17
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_obs   1.035
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_restrained_S_obs      1.035
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_obs          0.0530
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0170P)²+15.2729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1470
_refine_ls_wR_factor_obs         0.1199
_reflns_number_observed          2995
_reflns_number_total             3731
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960454q_3.cif
_cod_data_source_block           '[Ph4P]2[Zr2Ti2Cl16](3a)'
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+15.2729P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+15.2729P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323985
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zr1 Zr 0.06291(7) 0.13470(6) 0.34649(7) 0.0321(2) Uani 1 d . .
Ti1 Ti 0.07640(13) 0.38954(10) 0.52929(13) 0.0264(3) Uani 1 d . .
Cl1 Cl 0.0263(2) 0.22206(14) 0.5612(2) 0.0331(5) Uani 1 d . .
Cl2 Cl 0.2414(2) 0.29315(14) 0.4672(2) 0.0309(4) Uani 1 d . .
Cl3 Cl -0.0658(2) 0.29025(15) 0.2867(2) 0.0351(5) Uani 1 d . .
Cl4 Cl 0.2107(2) 0.4556(2) 0.7501(2) 0.0489(6) Uani 1 d . .
Cl5 Cl 0.1992(2) 0.0262(2) 0.4652(2) 0.0421(5) Uani 1 d . .
Cl6 Cl 0.1157(2) 0.53521(14) 0.4560(2) 0.0345(5) Uani 1 d . .
Cl7 Cl -0.1359(2) 0.0262(2) 0.2403(2) 0.0531(6) Uani 1 d . .
Cl8 Cl 0.1179(3) 0.0922(2) 0.1625(2) 0.0581(6) Uani 1 d . .
P1 P 0.3416(2) 0.70520(14) 0.2361(2) 0.0255(5) Uani 1 d . .
C11 C 0.1683(7) 0.6969(5) 0.1363(7) 0.024(2) Uani 1 d . .
C12 C 0.1099(8) 0.6138(6) 0.0178(8) 0.037(2) Uani 1 d . .
H12 H 0.1593(8) 0.5606(6) -0.0045(8) 0.045 Uiso 1 calc R .
C13 C -0.0192(9) 0.6097(8) -0.0660(9) 0.049(2) Uani 1 d . .
H13 H -0.0589(9) 0.5544(8) -0.1467(9) 0.059 Uiso 1 calc R .
C14 C -0.0901(8) 0.6871(8) -0.0310(9) 0.054(3) Uani 1 d . .
H14 H -0.1788(8) 0.6847(8) -0.0886(9) 0.065 Uiso 1 calc R .
C15 C -0.0340(9) 0.7678(8) 0.0864(10) 0.058(3) Uani 1 d . .
H15 H -0.0850(9) 0.8184(8) 0.1109(10) 0.069 Uiso 1 calc R .
C16 C 0.0967(8) 0.7749(7) 0.1683(8) 0.045(2) Uani 1 d . .
H16 H 0.1367(8) 0.8327(7) 0.2458(8) 0.054 Uiso 1 calc R .
C21 C 0.3814(7) 0.7804(5) 0.4086(7) 0.023(2) Uani 1 d . .
C22 C 0.3046(7) 0.7613(6) 0.4700(8) 0.032(2) Uani 1 d . .
H22 H 0.2308(7) 0.7119(6) 0.4199(8) 0.039 Uiso 1 calc R .
C23 C 0.3361(8) 0.8148(6) 0.6048(8) 0.037(2) Uani 1 d . .
H23 H 0.2852(8) 0.8010(6) 0.6470(8) 0.045 Uiso 1 calc R .
C24 C 0.4430(8) 0.8886(7) 0.6761(7) 0.038(2) Uani 1 d . .
H24 H 0.4642(8) 0.9266(7) 0.7669(7) 0.045 Uiso 1 calc R .
C25 C 0.5189(7) 0.9065(6) 0.6145(7) 0.032(2) Uani 1 d . .
H25 H 0.5933(7) 0.9551(6) 0.6649(7) 0.038 Uiso 1 calc R .
C26 C 0.4881(7) 0.8552(6) 0.4826(7) 0.030(2) Uani 1 d . .
H26 H 0.5391(7) 0.8703(6) 0.4412(7) 0.036 Uiso 1 calc R .
C31 C 0.3917(7) 0.5758(6) 0.2320(7) 0.028(2) Uani 1 d . .
C32 C 0.3850(9) 0.5284(7) 0.3244(8) 0.043(2) Uani 1 d . .
H32 H 0.3581(9) 0.5647(7) 0.3910(8) 0.051 Uiso 1 calc R .
C33 C 0.4184(9) 0.4269(6) 0.3169(8) 0.045(2) Uani 1 d . .
H33 H 0.4115(9) 0.3943(6) 0.3777(8) 0.054 Uiso 1 calc R .
C34 C 0.4607(8) 0.3737(6) 0.2242(9) 0.045(2) Uani 1 d . .
H34 H 0.4875(8) 0.3065(6) 0.2232(9) 0.054 Uiso 1 calc R .
C35 C 0.4634(11) 0.4209(7) 0.1314(11) 0.061(3) Uani 1 d . .
H35 H 0.4880(11) 0.3838(7) 0.0632(11) 0.073 Uiso 1 calc R .
C36 C 0.4311(10) 0.5206(6) 0.1372(9) 0.051(3) Uani 1 d . .
H36 H 0.4361(10) 0.5517(6) 0.0743(9) 0.061 Uiso 1 calc R .
C41 C -0.4239(7) 0.2342(6) -0.1646(7) 0.027(2) Uani 1 d . .
C42 C -0.3543(8) 0.1886(6) -0.0615(7) 0.035(2) Uani 1 d . .
H42 H -0.2634(8) 0.1897(6) -0.0284(7) 0.042 Uiso 1 calc R .
C43 C -0.4196(8) 0.1422(6) -0.0086(8) 0.039(2) Uani 1 d . .
H43 H -0.3725(8) 0.1115(6) 0.0606(8) 0.047 Uiso 1 calc R .
C44 C -0.5530(8) 0.1399(6) -0.0556(8) 0.036(2) Uani 1 d . .
H44 H -0.5965(8) 0.1083(6) -0.0185(8) 0.044 Uiso 1 calc R .
C45 C -0.6221(8) 0.1849(6) -0.1579(8) 0.040(2) Uani 1 d . .
H45 H -0.7132(8) 0.1823(6) -0.1916(8) 0.047 Uiso 1 calc R .
C46 C -0.5592(8) 0.2328(6) -0.2103(7) 0.034(2) Uani 1 d . .
H46 H -0.6069(8) 0.2651(6) -0.2774(7) 0.040 Uiso 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'
Ti Ti 0.2776 0.4457 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl8 Zr1 Cl5 97.13(9) . . y
Cl8 Zr1 Cl7 97.87(9) . . y
Cl5 Zr1 Cl7 99.15(8) . . y
Cl8 Zr1 Cl3 96.00(8) . . y
Cl5 Zr1 Cl3 163.31(7) . . y
Cl7 Zr1 Cl3 89.19(8) . . y
Cl8 Zr1 Cl1 167.41(8) . . y
Cl5 Zr1 Cl1 88.15(7) . . y
Cl7 Zr1 Cl1 92.53(8) . . y
Cl3 Zr1 Cl1 77.00(6) . . y
Cl8 Zr1 Cl2 89.35(8) . . y
Cl5 Zr1 Cl2 93.20(7) . . y
Cl7 Zr1 Cl2 164.76(8) . . y
Cl3 Zr1 Cl2 76.67(6) . . y
Cl1 Zr1 Cl2 78.91(6) . . y
Cl8 Zr1 Ti1 121.74(7) . . y
Cl5 Zr1 Ti1 116.87(6) . . y
Cl7 Zr1 Ti1 119.37(7) . . y
Cl3 Zr1 Ti1 46.78(5) . . y
Cl1 Zr1 Ti1 46.08(5) . . y
Cl2 Zr1 Ti1 46.08(5) . . y
Cl4 Ti1 Cl6 96.28(9) . 2_566 y
Cl4 Ti1 Cl6 97.10(9) . . y
Cl6 Ti1 Cl6 89.13(8) 2_566 . y
Cl4 Ti1 Cl1 92.20(9) . . y
Cl6 Ti1 Cl1 94.35(8) 2_566 . y
Cl6 Ti1 Cl1 169.66(9) . . y
Cl4 Ti1 Cl2 95.08(9) . . y
Cl6 Ti1 Cl2 168.49(9) 2_566 . y
Cl6 Ti1 Cl2 91.26(7) . . y
Cl1 Ti1 Cl2 83.39(7) . . y
Cl4 Ti1 Cl3 171.76(9) . . y
Cl6 Ti1 Cl3 88.15(8) 2_566 . y
Cl6 Ti1 Cl3 89.89(8) . . y
Cl1 Ti1 Cl3 80.51(7) . . y
Cl2 Ti1 Cl3 80.35(7) . . y
Cl4 Ti1 Zr1 123.24(8) . . y
Cl6 Ti1 Zr1 121.80(7) 2_566 . y
Cl6 Ti1 Zr1 121.40(7) . . y
Cl1 Ti1 Zr1 48.81(5) . . y
Cl2 Ti1 Zr1 49.07(5) . . y
Cl3 Ti1 Zr1 48.74(5) . . y
Cl4 Ti1 Ti1 99.41(8) . 2_566 y
Cl6 Ti1 Ti1 44.60(5) 2_566 2_566 y
Cl6 Ti1 Ti1 44.53(5) . 2_566 y
Cl1 Ti1 Ti1 138.08(8) . 2_566 y
Cl2 Ti1 Ti1 134.64(8) . 2_566 y
Cl3 Ti1 Ti1 88.62(7) . 2_566 y
Zr1 Ti1 Ti1 137.34(6) . 2_566 y
Ti1 Cl1 Zr1 85.11(7) . . y
Ti1 Cl2 Zr1 84.85(7) . . y
Ti1 Cl3 Zr1 84.48(6) . . y
Ti1 Cl6 Ti1 90.87(8) 2_566 . y
C41 P1 C21 110.7(3) 2_565 . ?
C41 P1 C31 108.5(3) 2_565 . ?
C21 P1 C31 109.5(3) . . ?
C41 P1 C11 109.1(3) 2_565 . ?
C21 P1 C11 109.2(3) . . ?
C31 P1 C11 109.9(3) . . ?
C16 C11 C12 120.0(7) . . ?
C16 C11 P1 121.2(6) . . ?
C12 C11 P1 118.5(5) . . ?
C13 C12 C11 120.0(8) . . ?
C12 C13 C14 119.2(8) . . ?
C15 C14 C13 121.1(8) . . ?
C14 C15 C16 120.1(9) . . ?
C11 C16 C15 119.4(8) . . ?
C26 C21 C22 119.3(7) . . ?
C26 C21 P1 121.7(5) . . ?
C22 C21 P1 119.0(6) . . ?
C23 C22 C21 120.4(7) . . ?
C24 C23 C22 119.1(7) . . ?
C23 C24 C25 120.1(7) . . ?
C26 C25 C24 121.1(8) . . ?
C25 C26 C21 120.0(7) . . ?
C36 C31 C32 118.5(7) . . ?
C36 C31 P1 121.8(6) . . ?
C32 C31 P1 119.6(6) . . ?
C33 C32 C31 119.3(8) . . ?
C34 C33 C32 121.6(8) . . ?
C33 C34 C35 118.2(8) . . ?
C36 C35 C34 120.9(8) . . ?
C31 C36 C35 121.3(8) . . ?
C42 C41 C46 118.8(7) . . ?
C42 C41 P1 120.7(6) . 2_565 ?
C46 C41 P1 120.5(5) . 2_565 ?
C43 C42 C41 119.7(7) . . ?
C44 C43 C42 121.0(7) . . ?
C43 C44 C45 119.3(7) . . ?
C46 C45 C44 120.6(8) . . ?
C45 C46 C41 120.5(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 Cl8 2.341(2) . y
Zr1 Cl5 2.351(2) . y
Zr1 Cl7 2.364(2) . y
Zr1 Cl3 2.590(2) . y
Zr1 Cl1 2.590(2) . y
Zr1 Cl2 2.601(2) . y
Zr1 Ti1 3.429(2) . y
Ti1 Cl4 2.241(2) . y
Ti1 Cl6 2.431(2) 2_566 y
Ti1 Cl6 2.435(2) . y
Ti1 Cl1 2.479(2) . y
Ti1 Cl2 2.480(2) . y
Ti1 Cl3 2.511(2) . y
Ti1 Ti1 3.467(3) 2_566 y
Cl6 Ti1 2.431(2) 2_566 ?
P1 C41 1.796(7) 2_565 ?
P1 C21 1.798(7) . ?
P1 C31 1.800(7) . ?
P1 C11 1.803(7) . ?
C11 C16 1.37(1) . ?
C11 C12 1.39(1) . ?
C12 C13 1.37(1) . ?
C13 C14 1.37(1) . ?
C14 C15 1.37(1) . ?
C15 C16 1.37(1) . ?
C21 C26 1.39(1) . ?
C21 C22 1.39(1) . ?
C22 C23 1.39(1) . ?
C23 C24 1.38(1) . ?
C24 C25 1.38(1) . ?
C25 C26 1.36(1) . ?
C31 C36 1.36(1) . ?
C31 C32 1.39(1) . ?
C32 C33 1.39(1) . ?
C33 C34 1.35(1) . ?
C34 C35 1.38(1) . ?
C35 C36 1.36(1) . ?
C41 C42 1.40(1) . ?
C41 C46 1.40(1) . ?
C41 P1 1.797(7) 2_565 ?
C42 C43 1.38(1) . ?
C43 C44 1.38(1) . ?
C44 C45 1.39(1) . ?
C45 C46 1.37(1) . ?
