Pseudo electron-deficient organometallics: limited reactivity towards electron-donating ligands
Pitto-Barry, Anaïs; Lupan, Alexandru; Zegke, Markus; Swift, Thomas; Attia, Amr A. A.; Lord, Rianne M.; Barry, Nicolas P. E.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02827J

data_7044277
_publ_section_title
;
 Pseudo electron-deficient organometallics: limited reactivity towards
 electron-donating ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02827J
_journal_year                    2017
_chemical_formula_moiety         'C16 H17 Cl2 Ir S2'
_chemical_formula_sum            'C16 H17 Cl2 Ir S2'
_chemical_formula_weight         536.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-08-29 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.4853(7)
_cell_length_b                   13.8473(13)
_cell_length_c                   29.535(2)
_cell_measurement_reflns_used    3170
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      66.38
_cell_measurement_theta_min      2.99
_cell_volume                     3470.3(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker SMART APEX2 (BRuker, 2012)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1286
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22761
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        63.684
_diffrn_reflns_theta_max         63.684
_diffrn_reflns_theta_min         2.992
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.887
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.3778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1349 before and 0.0957 after correction. The Ratio of minimum to maximum transmission is 0.5018. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       needle
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          1.072
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.787
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2843
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0574P)^2^+24.6675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2158
_reflns_number_total             2843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02827j2.cif
_cod_data_source_block           compound8
_cod_database_code               7044277
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.345
_shelx_estimated_absorpt_t_min   0.017
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Me refined with riding coordinates:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
;
_shelx_res_checksum              84132
_olex2_submission_special_instructions 'No special instructions were received'