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_4322834
_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 H20 O3 P Ru, C F3 S O3'
_chemical_formula_sum            'C17 H20 F3 O6 P Ru2 S'
_chemical_formula_weight         642.50
_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                 111.930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7600(10)
_cell_length_b                   11.2880(10)
_cell_length_c                   16.691(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      33.005
_cell_measurement_theta_min      19.752
_cell_volume                     2230.1(4)
_computing_cell_refinement       'XSCANS (Siemens, 1994)'
_computing_data_collection       'XSCANS (Siemens, 1994)'
_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      213(2)
_diffrn_measurement_device       'Siemens P4RA'
_diffrn_measurement_method       2\q-'\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3877
_diffrn_reflns_theta_max         56.74
_diffrn_reflns_theta_min         3.73
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.041
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_process_details   'XEMP (Siemens, 1990)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.00050(7)
_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   1.036
_refine_ls_goodness_of_fit_obs   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         2984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_obs          0.0410
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+3.0754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1088
_refine_ls_wR_factor_obs         0.1072
_reflns_number_observed          2730
_reflns_number_total             2984
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971516v_2.cif
_cod_data_source_block           str1164
_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^)+(0.0744P)^2^+3.0754P] 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^)+(0.0744P)^2^+3.0754P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4322834