Diphosphine Mobility at a Binuclear Metal Center: A Concerted Double Trigonal-Twist in Bis(dithiolate) Complexes [M2(CO)4(μ-dppm){μ-S(CH2)nS}] (M = Fe, Ru;n= 2, 3)
Hogarth, Graeme; Kabir, Shariff E.; Richards, Idris; Organometallics 29 (2010) 6559–; doi:10.1021/om100894w

data_4067197
_publ_section_title
;
 Diphosphine Mobility at a Binuclear Metal Center: A Concerted Double
 Trigonal-Twist in Bis(dithiolate) Complexes
 [M2(CO)4(\m-dppm){\m-S(CH2)nS}] (M = Fe, Ru;n= 2, 3)
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6559
_journal_paper_doi               10.1021/om100894w
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C31 H28 Fe2 O4 P2 S2'
_chemical_formula_weight         702.29
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.8100(10)
_cell_angle_beta                 84.1790(10)
_cell_angle_gamma                73.6400(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2906(6)
_cell_length_b                   10.9286(8)
_cell_length_c                   15.8512(11)
_cell_measurement_temperature    123(2)
_cell_volume                     1507.93(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12339
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.6993
_exptl_absorpt_correction_T_min  0.6496
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0440P)^2^+0.7297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                5956
_reflns_number_total             6613
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om100894w_si_001.cif
_cod_data_source_block           str0801
_cod_original_sg_symbol_H-M      P1bar
_cod_database_code               4067197