Disulfides of Manganese Carbonyl. Synthesis of Mn2(CO)7(μ-S2) and Its Reactions with Tertiary Phosphines and Arsines
Richard D. Adams; O-Sung Kwon; Mark D. Smith; Inorganic Chemistry 41 (2002) 6281–6290; doi:10.1021/ic0203670

data_4318898
_publ_section_title
;
 Disulfides of Manganese Carbonyl. Synthesis of Mn2(CO)7(\m-S2) and Its
 Reactions with Tertiary Phosphines and Arsines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6281
_journal_page_last               6290
_journal_paper_doi               10.1021/ic0203670
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C39 H35 Cl2 Mn4 O14 P3 S2'
_chemical_formula_weight         1175.36
_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                 99.457(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5722(13)
_cell_length_b                   21.011(3)
_cell_length_c                   21.996(3)
_cell_measurement_reflns_used    5463
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.029
_cell_measurement_theta_min      2.498
_cell_volume                     4819.6(11)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28370
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_T_max  0.894294
_exptl_absorpt_correction_T_min  0.700899
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         8534
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0730P)^2^+1.1059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                6372
_reflns_number_total             8534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203670_05.cif
_cod_data_source_block           kw3pme1s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318898