Serendipitous preparation of fac-(aceto-nitrile-κN)tri-chlorido-[(1,2,5,6-η)-cyclo-octa-1,5-diene]iridium(III).
Morris, David M.; Merola, Joseph S.; Acta crystallographica. Section E, Crystallographic communications 71 (2015) 371–373; doi:10.1107/S2056989015004855

data_2311279
_publ_section_title
;
 Serendipitous preparation of
 fac-(aceto-nitrile-\kN)tri-chlorido-[(1,2,5,6-\h)-cyclo-octa-1,5-diene]iridium(III).
;
_journal_coeditor_code           PK2547
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              371
_journal_page_last               373
_journal_paper_doi               10.1107/S2056989015004855
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ir Cl3 (C2 H3 N) (C8 H12)]'
_chemical_formula_moiety         'C10 H15 Cl3 Ir N'
_chemical_formula_sum            'C10 H15 Cl3 Ir N'
_chemical_formula_weight         447.78
_chemical_name_systematic
<i>fac</i>-(Acetonitrile-\k<i>N</i>)trichlorido[(1,2,5,6-\h)-cycloocta-1,5-diene]iridium(III)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.25131(10)
_cell_length_b                   11.85605(14)
_cell_length_c                   12.94150(15)
_cell_measurement_reflns_used    12030
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      32.1810
_cell_measurement_theta_min      3.9950
_cell_volume                     1266.04(3)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      99.8(4)
_diffrn_detector_area_resol_mean 16.0122
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur Eos Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27207
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.438
_diffrn_reflns_theta_min         3.437
_exptl_absorpt_coefficient_mu    11.146
_exptl_absorpt_correction_T_max  0.396
_exptl_absorpt_correction_T_min  0.204
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(SCALE3 ABSPACK; Clark & Reid, 1995)
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    2.349
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.2225
_exptl_crystal_size_mid          0.1454
_exptl_crystal_size_min          0.1111
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.742
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1715 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         4333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+1.2315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0368
_refine_ls_wR_factor_ref         0.0375
_reflns_number_gt                4173
_reflns_number_total             4333
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2547sup1.cif
_cod_data_source_block           I
_cod_database_code               2311279
_shelx_hkl_checksum              3908
_shelx_res_checksum              85742