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_4076749
_publ_section_title
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 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;
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_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            'C56 H84 O8 S4 Zr2'
_chemical_formula_weight         1195.91
_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                87.781(4)
_cell_angle_beta                 83.709(4)
_cell_angle_gamma                71.316(4)
_cell_formula_units_Z            1
_cell_length_a                   9.012(2)
_cell_length_b                   9.454(2)
_cell_length_c                   17.750(4)
_cell_measurement_reflns_used    1200
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.15
_cell_volume                     1424.0(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    'DIRDIF-96 (P. T. Beurskens)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_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  0.0828
_diffrn_reflns_av_sigmaI/netI    0.1006
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14926
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.9724
_exptl_absorpt_correction_T_min  0.8956
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.041
_refine_diff_density_min         -1.373
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6747
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.1006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+14.8657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2666
_refine_ls_wR_factor_ref         0.2884
_reflns_number_gt                4272
_reflns_number_total             6747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0110336.cif
_cod_data_source_block           c834_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        1423.9(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076749