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_4076748
_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            'C52 H76 O8 S2 Zr2'
_chemical_formula_weight         1075.69
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.5430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1148(8)
_cell_length_b                   9.3002(4)
_cell_length_c                   32.6894(15)
_cell_measurement_reflns_used    1200
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      1.22
_cell_volume                     5058.5(4)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            30577
_diffrn_reflns_theta_full        27.05
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.9474
_exptl_absorpt_correction_T_min  0.8111
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         10971
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                6926
_reflns_number_total             10971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0110336.cif
_cod_data_source_block           c742_fin
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      P2(1)/c
_cod_database_code               4076748