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_4323982
_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            'C79 H176 Ba2 Cd2 O24 Ti4'
_chemical_formula_weight         2201.28
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.83(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.677(20)
_cell_length_b                   12.603(11)
_cell_length_c                   18.996(20)
_cell_measurement_temperature    293(2)
_cell_volume                     5390(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       'Image plate'
_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    0.0845
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8873
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_F_000             2276
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.280
_refine_ls_goodness_of_fit_obs   1.416
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.280
_refine_ls_restrained_S_obs      1.416
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_obs          0.0880
_refine_ls_shift/esd_max         3.039
_refine_ls_shift/esd_mean        0.105
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+4.0333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2216
_refine_ls_wR_factor_obs         0.2069
_reflns_number_observed          6409
_reflns_number_total             8873
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960116p_3.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+4.0333P] 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^)+(0.0777P)^2^+4.0333P] 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        5390.4(88)
_cod_original_formula_sum        'C72 H168 Ba2 Cd2 O24 Ti4 * C7 H8'
_cod_database_code               4323982