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_4080310
_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         'C29 H66 Cd O11 Zr2'
_chemical_formula_sum            'C29 H66 Cd O11 Zr2'
_chemical_formula_weight         885.67
_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-97
_cell_angle_alpha                76.331(2)
_cell_angle_beta                 89.826(2)
_cell_angle_gamma                87.142(2)
_cell_formula_units_Z            6
_cell_length_a                   9.6602(2)
_cell_length_b                   24.5946(6)
_cell_length_c                   26.7211(6)
_cell_measurement_reflns_used    97435
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.43
_cell_volume                     6160.9(2)
_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      170(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'IPDS 2 T (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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            94984
_diffrn_reflns_theta_full        26.82
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         2.43
_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    1.057
_exptl_absorpt_correction_T_max  0.9430
_exptl_absorpt_correction_T_min  0.7115
_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    1.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       'not measured'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         26079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.083
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+4.1809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                20434
_reflns_number_total             26079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301053b_si_002.cif
_cod_data_source_block           6
_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 
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_cod_database_code               4080310