Protonation of Metal-Metal Bonds in Cp~2~Ru~2~(Co)~3~(PR~3~) and Cp~2~Mo~2~(CO)~4~(PR~3~)~2~
Chip Nataro; Robert J. Angelici; Inorganic Chemistry 37 (1998) 2975–2983; doi:10.1021/ic971516v

data_4322833
_publ_contact_author
;Prof. Robert J. Angelici
Department of Chemistry
Iowa State University
Ames, IA 50010
;
_publ_contact_author_email       angelici@iastate.edu
_publ_contact_author_fax         515-294-0105
_publ_contact_author_phone       515-294-2603
_publ_section_title
;
 Protonation of Metal-Metal Bonds in Cp~2~Ru~2~(Co)~3~(PR~3~) and
 Cp~2~Mo~2~(CO)~4~(PR~3~)~2~
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2975
_journal_page_last               2983
_journal_paper_doi               10.1021/ic971516v
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthetic
_chemical_formula_moiety         'C16 H19 O3 P Ru2'
_chemical_formula_sum            'C16 H19 O3 P Ru2'
_chemical_formula_weight         492.42
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.18(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.997(5)
_cell_length_b                   14.401(10)
_cell_length_c                   15.460(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.6
_cell_measurement_theta_min      7.2
_cell_volume                     1747(2)
_computing_cell_refinement       'P3/V release 4.21 (Siemens, 1990)'
_computing_data_collection       'P3/V release 4.21 (Siemens, 1990)'
_computing_data_reduction        'SHELXTL-Plus V4.0 (Siemens, 1990)'
_computing_molecular_graphics    'SHELXTL-Plus V4.0 (Siemens, 1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-Plus V4.0 (Siemens, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4RA'
_diffrn_measurement_method       2\q-\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_sigmaI/netI    0.2836
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6577
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.60
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.865
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.692
_refine_ls_goodness_of_fit_obs   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         5130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.692
_refine_ls_restrained_S_obs      0.987
_refine_ls_R_factor_all          0.1956
_refine_ls_R_factor_obs          0.0558
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1181
_refine_ls_wR_factor_obs         0.0914
_reflns_number_observed          1632
_reflns_number_total             5130
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971516v_1.cif
_cod_data_source_block           str1153
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1746.7(21)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4322833