Reactivity of the Organometallic fac-[(CO)3ReI(H2O)3]+ Aquaion. Kinetic and Thermodynamic Properties of H2O Substitution
Bernadette Salignac; Pascal V. Grundler; Sonia Cayemittes; Urban Frey; Rosario Scopelliti; André E. Merbach; Roman Hedinger; Kaspar Hegetschweiler; Roger Alberto; Ulrich Prinz; Gerhard Raabe; Ulrich Kölle; Syd Hall; Inorganic Chemistry 42 (2003) 3516–3526; doi:10.1021/ic0341744

data_4313738
_publ_section_title
;
 Reactivity of the Organometallic fac-[(CO)3ReI(H2O)3]+ Aquaion. Kinetic
 and Thermodynamic Properties of H2O Substitution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3516
_journal_page_last               3526
_journal_paper_doi               10.1021/ic0341744
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '2(C15 H10 N2 O4 Re), C F3 O3 S, N O3, 2(H2 O)'
_chemical_formula_sum            'C31 H24 F3 N5 O16 Re2 S'
_chemical_formula_weight         1184.02
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.764(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.413(3)
_cell_length_b                   22.156(3)
_cell_length_c                   12.5038(16)
_cell_measurement_reflns_used    3633
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      23.21115
_cell_measurement_theta_min      1.5282
_cell_volume                     3650.5(11)
_computing_cell_refinement       'Oxford Diffraction, CrysAlis RED'
_computing_data_collection       'marresearch, mar345'
_computing_data_reduction        'Oxford Diffraction, CrysAlis RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'marresearch mar345 IPDS'
_diffrn_measurement_method
'60 images with deltaphi = 3 deg and exp. time = 180 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26642
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    6.780
_exptl_absorpt_correction_T_max  0.7060
_exptl_absorpt_correction_T_min  0.2480
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.039
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.216
_refine_ls_extinction_coef       0.00053(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_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0683P)^2^+0.8874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                6591
_reflns_number_total             8449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0341744si20030217_060152.cif
_cod_data_source_block           merb48
_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 

2020-10-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         592.01
_cod_original_formula_moiety
'C15 H10 N2 O4 Re, 0.5(C F3 O3 S), 0.5(N O3), H2 O'
_cod_original_formula_units_Z            8
_cod_original_cell_volume        3650.3(9)
_cod_original_formula_sum        'C15.50 H12 F1.50 N2.50 O8 Re S0.50'
_cod_database_code               4313738