The rational synthesis of tetranuclear heterometallic butterfly clusters: reactions of [M2(CO)6(μ-pyS)2] (M = Re, Mn) with group VIII metal carbonyls
Ghosh, Shishir; Khanam, Kamrun N.; Hossain, G. M. Golzar; Haworth, Daniel T.; Lindeman, Sergey V.; Hogarth, Graeme; Kabir, Shariff E.; New Journal of Chemistry 34 (2010) 1875–; doi:10.1039/b9nj00526a

data_7053353
_publ_section_title
;
 The rational synthesis of tetranuclear heterometallic butterfly clusters:
 reactions of [M2(CO)6(\m-pyS)2] (M = Re, Mn) with group VIII metal
 carbonyls
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1875
_journal_paper_doi               10.1039/b9nj00526a
_journal_volume                  34
_journal_year                    2010
_chemical_formula_sum            'C35 H19 N O12 Os3 P Re S'
_chemical_formula_weight         1465.34
_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                 98.3000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1359(13)
_cell_length_b                   15.1378(15)
_cell_length_c                   18.6633(19)
_cell_measurement_reflns_used    8212
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.5
_cell_volume                     3672.3(6)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_data_reduction        'SADABS-2004/1 (Bruker, 2005)'
_computing_molecular_graphics    'XP v5.1 (Bruker, 1998)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'XL/SHELXTL v6.10 (Bruker, 2001)'
_computing_structure_solution    'XS/SHELXTL v6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       'omega scan'
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            60539
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.02
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    13.797
_exptl_absorpt_correction_T_max  0.5756
_exptl_absorpt_correction_T_min  0.0923
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Numerical (based on real shape of the crystal) absorption
correction followed by:
SADABS. Program for empirical absorption correction of
area-detector data. University of Goetingen. Germany.
Sheldrick, G. M. 1996
;
_exptl_crystal_colour            purple-red
_exptl_crystal_density_diffrn    2.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.619
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         12142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+3.0630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0443
_reflns_number_gt                10783
_reflns_number_total             12142
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00526a.txt
_cod_data_source_block           dthf
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               7053353