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)
Michael Veith; Sanjay Mathur; Volker Huch; Inorganic Chemistry 35 (1996) 7295–7303; doi:10.1021/ic960116p

data_4323981
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0560P)^2^+3.2511P] where P=(Fo^2^+2Fc^2^)/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