A new polymorph of [(<i>S</i>)-({-})-2-aminomethyl-1-ethylpyrrolidine-κ^2^<i>N,N</i>'](1,5-cyclooctadiene)rhodium(I) trifluoromethanesulfonate
Jones, Matthew D.; Almeida Paz, Filipe A.; Davies, John E.; Johnson, Brian F. G.; Klinowski, Jacek; Acta Crystallographica Section E 59 (2003) m1091–m1093; doi:10.1107/S1600536803024760

data_2202452
_publ_section_title
;A new polymorph of
 [(<i>S</i>)-({-})-2-aminomethyl-1-ethylpyrrolidine-\k^2^<i>N,N</i>'](1,5-cyclooctadiene)rhodium(I)
 trifluoromethanesulfonate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1091
_journal_page_last               m1093
_journal_paper_doi               10.1107/S1600536803024760
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Rh (C8 H12) (C7 H16 N2)] C F3 S O3'
_chemical_formula_moiety         'C15 H28 N2 Rh, C F3 O3 S'
_chemical_formula_sum            'C16 H28 F3 N2 O3 Rh S'
_chemical_formula_weight         488.37
_chemical_name_systematic
;
[(S)-(-)-2-aminomethyl-1-ethylpyrrolidine-
\k^2^N,N'](1,5-cyclooctadiene)rhodium(I) trifluoromethanesulfonate
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.7449(5)
_cell_length_b                   14.5747(7)
_cell_length_c                   22.9700(12)
_cell_measurement_reflns_used    53723
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      21.97
_cell_measurement_theta_min      1.02
_cell_volume                     3932.0(3)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Thin-slice \w and \f'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6274
_diffrn_reflns_theta_full        21.96
_diffrn_reflns_theta_max         21.96
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.377
_refine_ls_abs_structure_details 'Flack (1983), 878 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.06(8)
_refine_ls_extinction_coef       0.0014(2)
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2212
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0477P)^2^+8.7148P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                2004
_reflns_number_total             2212
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6296.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2202452
_cod_database_fobs_code          2202452