Evaluation of Triflate Displacement by Water in CH2Cl2 Solution: Comparison of trans-[Rh(CO)(PPh3)2(OSO2CF3)] and the Crystalline Salt trans-[Rh(CO)(PPh3)2(OH2)][OTf]
Anna Svetlanova-Larsen; John L. Hubbard; Inorganic Chemistry 35 (1996) 3073–3076; doi:10.1021/ic951287h

data_4323812
_publ_section_title
;
 Evaluation of Triflate Displacement by Water in CH2Cl2 Solution:
 Comparison of trans-[Rh(CO)(PPh3)2(OSO2CF3)] and the Crystalline Salt
 trans-[Rh(CO)(PPh3)2(OH2)][OTf]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3073
_journal_page_last               3076
_journal_paper_doi               10.1021/ic951287h
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source        synthesis
_chemical_formula_analytical     'C38 H32 O5 F3 S P2 Rh '
_chemical_formula_sum            'C38 H30 F3 O4 P2 Rh S'
_chemical_formula_weight         804.53
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.03(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.401(8)
_cell_length_b                   9.122(4)
_cell_length_c                   17.047(6)
_cell_measurement_reflns_used    2283
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.5
_cell_volume                     3479(2)
_computing_cell_refinement       'Vax 3100'
_computing_data_collection       'Vax 3100 '
_computing_data_reduction        'Vax 3100'
_computing_molecular_graphics    'PC-based XP program'
_computing_publication_material  'PC-based SHELXL-93'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'theta- 2 theta '
_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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.2065
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2345
_diffrn_reflns_theta_max         22.56
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_density_meas      1.57
_exptl_crystal_density_method    'flotation in CCl4/ hexane'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       no
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.108
_refine_ls_goodness_of_fit_obs   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2278
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.123
_refine_ls_restrained_S_obs      1.217
_refine_ls_R_factor_all          0.2126
_refine_ls_R_factor_obs          0.1057
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+162.2319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2308
_refine_ls_wR_factor_obs         0.1740
_reflns_number_observed          1144
_reflns_number_total             2283
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951287h.cif
_cod_data_source_block           as23a_JL_HUBBARD/UTAH_STATE_UNIVERSITY
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+162.2319P] 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^)+(0.0010P)^2^+162.2319P] 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        3479.4(23)
_cod_database_code               4323812