Synthesis and Se−Se Bond Breaking of Polyselenides Containing Pendant Diphosphine Complexes of Manganese(I)†
Ruiz, Javier; Araúz, René; Ceroni, Mario; Vivanco, Marilín; Van der Maelen, Juan F.; García-Granda, Santiago; Organometallics 29 (2010) 3058–; doi:10.1021/om100229q

data_4065966
_publ_section_title
;
 Synthesis and Se&#x2212;Se Bond Breaking of Polyselenides Containing
 Pendant Diphosphine Complexes of Manganese(I)&#x2020;
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3058
_journal_paper_doi               10.1021/om100229q
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety
'C58 H42 Mn2 O8 P4 Se2, 2(Cl O4), 2(C H2 Cl2)'
_chemical_formula_sum            'C60 H46 Cl6 Mn2 O16 P4 Se2'
_chemical_formula_weight         1627.35
_chemical_name_common
'[(CO)4Mn(PPh2)2CH-Se2-CH(PPh2)2Mn(CO)4][ClO4]2&#x00B7;2[CH2Cl2]'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.01(3)
_cell_angle_beta                 82.40(4)
_cell_angle_gamma                68.94(2)
_cell_formula_units_Z            2
_cell_length_a                   11.742(4)
_cell_length_b                   15.627(4)
_cell_length_c                   20.587(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      14.45
_cell_measurement_theta_min      5.90
_cell_volume                     3313(2)
_computing_cell_refinement       'DIRDIF96 (Beurskens et al, 1996)'
_computing_data_collection       'CAD-4 Control Software (Nonius, 1994)'
_computing_data_reduction        'REFLEX (Local program, 1999)'
_computing_molecular_graphics    'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF96 (Beurskens et al, 1996)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius CAD4 Diffractometer'
_diffrn_measurement_method       '\w-2\q scan technique'
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.1054
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13366
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.05
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.884
_exptl_absorpt_correction_T_max  0.6886
_exptl_absorpt_correction_T_min  0.5989
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   semi-empirical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prysmatic
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.198
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         12982
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0470P)^2^+0.0404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                7010
_reflns_number_total             12982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100229q_si_001.cif
_cod_data_source_block           3-Se2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065966