Synthetic and Structural Investigations on the Reactivity of the Cd–I Bond in [ICd{Zr2(OPri)9}] to Construct New Mixed-Metal Alkoxides
Hegemann, Corinna; Tyrra, Wieland; Neudörfl, Jörg-Martin; Mathur, Sanjay; Organometallics 32 (2013) 1654–; doi:10.1021/om301053b

data_4080312
_publ_section_title
;
 Synthetic and Structural Investigations on the Reactivity of the Cd--I
 Bond in [ICd{Zr2(OPri)9}] to Construct New Mixed-Metal Alkoxides
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1654
_journal_paper_doi               10.1021/om301053b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C54 H126 Cd2 Cl2 O26 Zr4'
_chemical_formula_sum            'C54 H126 Cd2 Cl2 O26 Zr4'
_chemical_formula_weight         1852.13
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.021(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4431(13)
_cell_length_b                   19.5270(17)
_cell_length_c                   21.303(2)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.57
_cell_volume                     4238.9(8)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'IPDS II (Stoe & Cie)'
_diffrn_measurement_method       '\w and \f 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  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42396
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.9342
_exptl_absorpt_correction_T_min  0.7449
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correction (X-RED; Stoe & Cie, 2001)
was performed after optimizing the crystal shape
using X-SHAPE (Stoe & Cie, 1999).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00019(10)
_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_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                4405
_reflns_number_total             8205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301053b_si_002.cif
_cod_data_source_block           8
_cod_original_cell_volume        4238.9(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4080312