Low-temperature phase of diaqua(1,5-cyclooctadiene)rhodium(I) trifluoromethanesulfonate
Bats, Jan W.; Rivas Nass, Andreas; Hashmi, A. Stephen K.; Acta Crystallographica Section E 60 (2004) m85–m87; doi:10.1107/S160053680302823X

data_2203086
_publ_section_title
;
 Low-temperature phase of diaqua(1,5-cyclooctadiene)rhodium(I)
 trifluoromethanesulfonate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m85
_journal_page_last               m87
_journal_paper_doi               10.1107/S160053680302823X
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Rh (C8 H12) (H2 O1)2] (C F3 O3 S)'
_chemical_formula_moiety         'C8 H16 O2 Rh +, C F3 O3 S -'
_chemical_formula_sum            'C9 H16 F3 O5 Rh S'
_chemical_formula_weight         396.19
_chemical_name_systematic
;
diaqua(1,5-cyclooctadiene)rhodium(I) triflate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.944(12)
_cell_angle_beta                 105.414(10)
_cell_angle_gamma                116.683(10)
_cell_formula_units_Z            4
_cell_length_a                   11.9569(11)
_cell_length_b                   12.0716(17)
_cell_length_c                   12.1417(17)
_cell_measurement_reflns_used    177
_cell_measurement_temperature    152(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     1357.1(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      152(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Siemens SMART 1K CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.089
_diffrn_reflns_av_sigmaI/netI    0.067
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17620
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         30.2
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  600
_diffrn_standards_number         530
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.414
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.788
_refine_diff_density_min         -3.262
_refine_ls_extinction_coef       0.0052(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7851
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.07P)^2^+5P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                7426
_reflns_number_total             7851
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6278.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C9 H16 F3 O5 Rh1 S1'
_cod_database_code               2203086
_cod_database_fobs_code          2203086