(Diethylenetriamine-κ^3^<i>N</i>)(η^5^-pentamethylcyclopentadienyl)iridium(III) bis(trifluoromethanesulfonate)
Michael Scharwitz; Tobias van Almsick; William S. Sheldrick; Acta Crystallographica Section E 63 (2007) m537–m539; doi:10.1107/S1600536807002036

data_2212402
_publ_section_title
;(Diethylenetriamine-\k^3^<i>N</i>)(\h^5^-pentamethylcyclopentadienyl)iridium(III)
 bis(trifluoromethanesulfonate)
;
_journal_coeditor_code           WM2089
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m537
_journal_page_last               m539
_journal_paper_doi               10.1107/S1600536807002036
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ir (C10 H15) (C4 H13 N3)] (C F3 S O3)2'
_chemical_formula_moiety         'C14 H28 Ir N3 2+, 2(C F3 O3 S -)'
_chemical_formula_sum            'C16 H28 F6 Ir N3 O6 S2'
_chemical_formula_weight         728.73
_chemical_name_systematic
;
(Diethylenetriamine-\k^3^N)(\h^5^-pentamethylcyclopentadienyl)iridium(III)
bis(trifluoromethanesulfonate)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.244(2)
_cell_length_b                   13.733(3)
_cell_length_c                   17.869(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      20.31
_cell_measurement_theta_min      7.23
_cell_volume                     2513.8(9)
_computing_cell_refinement       R3m/V
_computing_data_collection       'R3m/V (Siemens, 1989)'
_computing_data_reduction        'XDISK (Siemens, 1989)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens P4 4-circle'
_diffrn_measurement_method       \w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2511
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0.01
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.558
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.057
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i> (1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.844
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.006(13)
_refine_ls_extinction_coef       0.0028(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     314
_refine_ls_number_reflns         2511
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.5443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0639
_reflns_number_gt                2335
_reflns_number_total             2511
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2089.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               2212402
_cod_database_fobs_code          2212402