Sequential Construction of One, Two, or Three Dithiolene Ligands from Alkynes and Sulfur in Dinuclear Cyclopentadienyl Molybdenum Complexes
Harry Adams; Matthew N. Bancroft; Michael J. Morris; Andrea E. Riddiough; Inorganic Chemistry 48 (2009) 9557–9566; doi:10.1021/ic901243m

data_4303305
_publ_contact_author_address
;
  Department of Chemistry
  University of Sheffield
  Sheffield
  S3 7HF
  UK
;
_publ_contact_author_email       m.morris@sheffield.ac.uk
_publ_contact_author_fax         '0114 222 9346'
_publ_contact_author_name        'Michael J. Morris*'
_publ_contact_author_phone       '0114 222 9363'
_publ_section_title
;
Sequential Construction of One, Two, or Three Dithiolene Ligands from
Alkynes and Sulfur in Dinuclear Cyclopentadienyl Molybdenum Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9557
_journal_page_last               9566
_journal_paper_doi               10.1021/ic901243m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C29 H32 Mo2 O13 S6'
_chemical_formula_weight         972.79
_chemical_name_systematic
;  
 ?  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.201(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8568(11)
_cell_length_b                   12.6101(10)
_cell_length_c                   21.3874(18)
_cell_measurement_reflns_used    2133
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.09
_cell_measurement_theta_min      2.12
_cell_volume                     3707.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0761
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23078
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.8300
_exptl_absorpt_correction_T_min  0.7247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0773P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                6002
_reflns_number_total             8950
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901243m_si_001_5.cif
_cod_data_source_block           ims34m
_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_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4303305