A novel organometallic macrocycle containing a tetrahedral Mo~2~Fe(μ~3~-S) cluster core
Guo, Dian-Shun; Gao, Yong-Hong; Zhang, Xiao-Ling; Ma, Jian-Ping; Acta Crystallographica Section E 62 (2006) m1285–m1286; doi:10.1107/S160053680601676X

data_2209078
_publ_section_title
;
 A novel organometallic macrocycle containing a tetrahedral
 Mo~2~Fe(\m~3~-S) cluster core
;
_journal_coeditor_code           BH2016
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1285
_journal_page_last               m1286
_journal_paper_doi               10.1107/S160053680601676X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mo2 Fe (C5 H6 O2) S (C O)7]'
_chemical_formula_moiety         'C22 H14 Fe Mo2 O9 S'
_chemical_formula_sum            'C22 H14 Fe Mo2 O9 S'
_chemical_formula_weight         702.12
_chemical_name_systematic
;
[\m~2~-\h^5^,\h^5^-1,1'-(propane-1,3-diyldicarbonyl)dicyclopentadienyl]-
\m~3~-thio-heptacarbonylirondimolybdenum(2 Fe---Mo, Mo---Mo)
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.255(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.123(2)
_cell_length_b                   18.835(4)
_cell_length_c                   12.326(2)
_cell_measurement_reflns_used    7955
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.911
_cell_measurement_theta_min      2.324
_cell_volume                     2267.3(8)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9389
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.866
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            'nut brown'
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.444
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0200
_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^)+(0.0277P)^2^+0.523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0510
_reflns_number_gt                3673
_reflns_number_total             3990
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2016.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2209078
_cod_database_fobs_code          2209078