#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:41:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179342 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/39/4323981.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_4323981
loop_
_publ_author_name
'Michael Veith'
'Sanjay Mathur'
'Volker Huch'
_publ_section_title
;
 Synthesis and Spectroscopic Characterization of Novel Heterotermetallic
 Isopropoxides: X-ray Crystal Structures of ICd{M2(OPri)9} and
 [{Cd(OPri)3}Ba{M2(OPri)9}]2 (M = Ti, Hf)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7295
_journal_page_last               7303
_journal_paper_doi               10.1021/ic960116p
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C27 H63 Cd Hf2 I O9'
_chemical_formula_weight         1128.05
_chemical_name_systematic
;
 ?
;
_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                95.619(12)
_cell_angle_beta                 99.915(11)
_cell_angle_gamma                111.347(11)
_cell_formula_units_Z            2
_cell_length_a                   9.825(2)
_cell_length_b                   11.428(2)
_cell_length_c                   20.619(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2091.3(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7684
_diffrn_reflns_theta_max         26.16
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    6.231
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.816
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.0122(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.261
_refine_ls_goodness_of_fit_obs   1.316
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.261
_refine_ls_restrained_S_obs      1.316
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_obs          0.0531
_refine_ls_shift/esd_max         -0.027
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0560P)²+3.2511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1445
_refine_ls_wR_factor_obs         0.1380
_reflns_number_observed          6481
_reflns_number_total             7684
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960116p_2.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+3.2511P] 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^)+(0.0560P)^2^+3.2511P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2091.3(6)
_cod_database_code               4323981
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
Hf1 Hf 0.42722(4) 0.67543(3) 0.31314(2) 0.0648(2) Uani 1 d . .
Hf2 Hf 0.40283(4) 0.78901(4) 0.17216(2) 0.0663(2) Uani 1 d . .
Cd Cd 0.69234(8) 0.94173(7) 0.29831(4) 0.0745(2) Uani 1 d . .
I I 0.94634(11) 1.13865(10) 0.34718(6) 0.1368(4) Uani 1 d . .
O1 O 0.5725(6) 0.7364(6) 0.2378(3) 0.0633(13) Uani 1 d . .
O2 O 0.4322(6) 0.8609(5) 0.2819(3) 0.0614(13) Uani 1 d . .
O3 O 0.2780(6) 0.6286(6) 0.2151(3) 0.076(2) Uani 1 d . .
O4 O 0.6267(7) 0.8021(6) 0.3718(3) 0.076(2) Uani 1 d . .
O5 O 0.5878(7) 0.9531(6) 0.1883(3) 0.082(2) Uani 1 d . .
O6 O 0.4548(10) 0.5189(7) 0.3184(4) 0.101(2) Uani 1 d . .
O7 O 0.2910(8) 0.6618(7) 0.3713(4) 0.089(2) Uani 1 d . .
O8 C 0.2490(9) 0.8484(9) 0.1402(4) 0.066(2) Uani 1 d . .
O9 C 0.4108(10) 0.7044(9) 0.0884(4) 0.065(2) Uani 1 d . .
C1 C 0.6724(14) 0.6741(12) 0.2218(7) 0.099(3) Uani 1 d . .
C2 C 0.5829(19) 0.5444(14) 0.1773(8) 0.120(5) Uani 1 d . .
C3 C 0.7890(18) 0.7546(17) 0.1935(11) 0.153(7) Uani 1 d . .
C4 C 0.3698(13) 0.9509(11) 0.3040(6) 0.091(3) Uani 1 d . .
C5 C 0.2021(16) 0.8824(15) 0.2978(8) 0.117(4) Uani 1 d . .
C6 C 0.4572(17) 1.0212(12) 0.3726(7) 0.111(4) Uani 1 d . .
C7 C 0.1412(15) 0.5230(17) 0.1870(10) 0.158(8) Uani 1 d . .
C8 C 0.1495(25) 0.4270(23) 0.1464(15) 0.230(14) Uani 1 d . .
C9 C 0.0310(20) 0.5115(21) 0.2149(16) 0.232(14) Uani 1 d . .
C10 C 0.7070(14) 0.7952(15) 0.4374(6) 0.103(4) Uani 1 d . .
C11 C 0.7308(18) 0.9127(19) 0.4851(7) 0.137(6) Uani 1 d . .
C12 C 0.8519(20) 0.7873(19) 0.4289(8) 0.153(7) Uani 1 d . .
C13 C 0.6322(14) 1.0496(12) 0.1473(6) 0.096(3) Uani 1 d . .
C14 C 0.6390(20) 1.1794(13) 0.1875(8) 0.127(5) Uani 1 d . .
C15 C 0.7808(20) 1.0659(16) 0.1338(8) 0.133(5) Uani 1 d . .
C16 C 0.4426(36) 0.3834(31) 0.3241(16) 0.250(17) Uani 1 d . .
C17 C 0.3956(41) 0.3639(30) 0.3844(21) 0.270(18) Uani 1 d . .
C18 C 0.6088(34) 0.4040(24) 0.3412(18) 0.230(13) Uani 1 d . .
C19 C 0.2013(23) 0.6400(22) 0.4178(9) 0.175(9) Uani 1 d . .
C20 C 0.2592(31) 0.7297(23) 0.4772(10) 0.208(12) Uani 1 d . .
C21 C 0.1126(55) 0.5280(30) 0.4147(20) 0.419(40) Uani 1 d . .
C22 C 0.1363(21) 0.8896(21) 0.1103(10) 0.166(8) Uani 1 d . .
C23 C 0.0444(30) 0.8032(28) 0.0519(13) 0.240(14) Uani 1 d . .
C24 C 0.1873(27) 1.0220(27) 0.1097(20) 0.255(18) Uani 1 d . .
C25 C 0.4147(21) 0.6557(20) 0.0242(7) 0.150(7) Uani 1 d . .
C26 C 0.2757(24) 0.5961(31) -0.0160(9) 0.231(14) Uani 1 d . .
C27 C 0.5398(28) 0.7369(27) -0.0002(10) 0.189(9) Uani 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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 '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
O6 Hf1 O7 99.8(3) . . ?
O6 Hf1 O4 100.2(3) . . ?
O7 Hf1 O4 102.6(3) . . ?
O6 Hf1 O3 100.9(3) . . ?
O7 Hf1 O3 101.8(3) . . ?
O4 Hf1 O3 144.2(2) . . ?
O6 Hf1 O2 162.6(3) . . ?
O7 Hf1 O2 97.3(3) . . ?
O4 Hf1 O2 78.8(2) . . ?
O3 Hf1 O2 72.5(2) . . ?
O6 Hf1 O1 95.3(3) . . ?
O7 Hf1 O1 164.6(3) . . ?
O4 Hf1 O1 77.0(2) . . ?
O3 Hf1 O1 72.5(2) . . ?
O2 Hf1 O1 67.5(2) . . ?
O8 Hf2 O9 99.0(4) . . ?
O8 Hf2 O5 100.7(3) . . ?
O9 Hf2 O5 101.4(3) . . ?
O8 Hf2 O3 100.6(3) . . ?
O9 Hf2 O3 101.5(3) . . ?
O5 Hf2 O3 145.6(2) . . ?
O8 Hf2 O1 163.9(3) . . ?
O9 Hf2 O1 96.9(3) . . ?
O5 Hf2 O1 79.1(2) . . ?
O3 Hf2 O1 73.0(2) . . ?
O8 Hf2 O2 96.2(3) . . ?
O9 Hf2 O2 164.6(3) . . ?
O5 Hf2 O2 78.6(2) . . ?
O3 Hf2 O2 72.6(2) . . ?
O1 Hf2 O2 67.9(2) . . ?
O4 Cd O1 71.4(2) . . ?
O4 Cd O2 72.4(2) . . ?
O1 Cd O2 65.8(2) . . ?
O4 Cd O5 135.8(2) . . ?
O1 Cd O5 71.6(2) . . ?
O2 Cd O5 71.0(2) . . ?
O4 Cd I 113.5(2) . . ?
O1 Cd I 147.53(14) . . ?
O2 Cd I 146.62(14) . . ?
O5 Cd I 110.7(2) . . ?
C1 O1 Hf2 131.8(6) . . ?
C1 O1 Hf1 122.5(6) . . ?
Hf2 O1 Hf1 93.6(2) . . ?
C1 O1 Cd 115.1(6) . . ?
Hf2 O1 Cd 92.2(2) . . ?
Hf1 O1 Cd 91.5(2) . . ?
C4 O2 Hf2 121.8(6) . . ?
C4 O2 Hf1 132.3(6) . . ?
Hf2 O2 Hf1 93.9(2) . . ?
C4 O2 Cd 115.4(6) . . ?
Hf2 O2 Cd 91.7(2) . . ?
Hf1 O2 Cd 91.6(2) . . ?
C7 O3 Hf2 130.4(10) . . ?
C7 O3 Hf1 130.4(10) . . ?
Hf2 O3 Hf1 99.1(2) . . ?
C10 O4 Hf1 129.4(7) . . ?
C10 O4 Cd 132.1(7) . . ?
Hf1 O4 Cd 98.1(2) . . ?
C13 O5 Hf2 130.8(7) . . ?
C13 O5 Cd 132.1(7) . . ?
Hf2 O5 Cd 97.0(2) . . ?
C16 O6 Hf1 167.9(12) . . ?
C19 O7 Hf1 171.5(12) . . ?
C22 O8 Hf2 174.7(11) . . ?
C25 O9 Hf2 172.9(11) . . ?
C3 C1 O1 111.8(11) . . ?
C3 C1 C2 112.3(13) . . ?
O1 C1 C2 110.7(10) . . ?
O2 C4 C6 109.0(9) . . ?
O2 C4 C5 109.9(10) . . ?
C6 C4 C5 115.0(11) . . ?
C9 C7 C8 124.0(17) . . ?
C9 C7 O3 117.0(16) . . ?
C8 C7 O3 116.4(16) . . ?
O4 C10 C12 107.6(11) . . ?
O4 C10 C11 107.7(11) . . ?
C12 C10 C11 112.2(13) . . ?
O5 C13 C15 110.2(10) . . ?
O5 C13 C14 107.3(10) . . ?
C15 C13 C14 110.5(12) . . ?
C17 C16 O6 103.5(22) . . ?
C17 C16 C18 104.4(28) . . ?
O6 C16 C18 100.7(23) . . ?
C21 C19 O7 117.1(21) . . ?
C21 C19 C20 122.7(20) . . ?
O7 C19 C20 115.0(16) . . ?
C23 C22 C24 119.4(22) . . ?
C23 C22 O8 110.5(18) . . ?
C24 C22 O8 114.4(17) . . ?
C26 C25 O9 112.2(16) . . ?
C26 C25 C27 121.6(18) . . ?
O9 C25 C27 113.6(15) . . ?
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
Hf1 O6 1.915(7) . ?
Hf1 O7 1.922(7) . ?
Hf1 O4 2.043(6) . ?
Hf1 O3 2.173(6) . ?
Hf1 O2 2.261(5) . ?
Hf1 O1 2.277(5) . ?
Hf2 O8 1.916(8) . ?
Hf2 O9 1.923(8) . ?
Hf2 O5 2.030(7) . ?
Hf2 O3 2.168(6) . ?
Hf2 O1 2.255(5) . ?
Hf2 O2 2.261(5) . ?
Cd O4 2.306(6) . ?
Cd O1 2.315(6) . ?
Cd O2 2.329(6) . ?
Cd O5 2.361(7) . ?
Cd I 2.6284(12) . ?
O1 C1 1.468(11) . ?
O2 C4 1.452(10) . ?
O3 C7 1.419(12) . ?
O4 C10 1.469(12) . ?
O5 C13 1.441(12) . ?
O6 C16 1.53(2) . ?
O7 C19 1.39(2) . ?
O8 C22 1.42(2) . ?
O9 C25 1.398(14) . ?
C1 C3 1.44(2) . ?
C1 C2 1.52(2) . ?
C4 C6 1.50(2) . ?
C4 C5 1.52(2) . ?
C7 C9 1.28(3) . ?
C7 C8 1.35(3) . ?
C10 C12 1.50(2) . ?
C10 C11 1.50(2) . ?
C13 C15 1.48(2) . ?
C13 C14 1.60(2) . ?
C16 C17 1.41(4) . ?
C16 C18 1.53(4) . ?
C19 C21 1.25(3) . ?
C19 C20 1.40(3) . ?
C22 C23 1.41(3) . ?
C22 C24 1.41(3) . ?
C25 C26 1.36(2) . ?
C25 C27 1.45(3) . ?
