Early-Transition-Metal Macrocycles as Metalloligands: Synthesis and Structure of Dinuclear Zirconocene Thioglycolates [Cp°2Zr{OOC(CH2SCH2)nCOO}2ZrCp°2] (n= 1, 2) and Their Heterobimetallic Complexes with Mo0and PdII ‡
Wenzel, Barbara; Lönnecke, Peter; Hey-Hawkins, Evamarie; Organometallics 21 (2002) 2070–; doi:10.1021/om0110336

data_4076750
_publ_section_title
;
 Early-Transition-Metal Macrocycles as Metalloligands:&#x00A0; Synthesis
 and Structure of Dinuclear Zirconocene Thioglycolates
 [Cp\%2Zr{OOC(CH2SCH2)nCOO}2ZrCp\%2] (n= 1, 2) and Their Heterobimetallic
 Complexes with Mo0and PdII&#x00A0;&#x2021;
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2070
_journal_paper_doi               10.1021/om0110336
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C68 H92 Mo2 O18 S2 Zr2'
_chemical_formula_weight         1635.86
_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                99.365(2)
_cell_angle_beta                 106.104(2)
_cell_angle_gamma                98.287(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8376(14)
_cell_length_b                   11.1310(16)
_cell_length_c                   17.628(3)
_cell_measurement_reflns_used    1200
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.07
_cell_measurement_theta_min      1.23
_cell_volume                     1793.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega 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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0762
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19407
_diffrn_reflns_theta_full        29.07
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.9635
_exptl_absorpt_correction_T_min  0.8646
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                5649
_reflns_number_total             8607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0110336.cif
_cod_data_source_block           c899_fin
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1792.9(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076750