Facile generation of iridium PCcarbeneP pincer complexes via water elimination from an alcohol proligand
Sung, Simon; Young, Rowan Drury; Dalton Trans.  (2017) –; doi:10.1039/C7DT03690F

data_7044525
_publ_section_title
;
 Facile generation of iridium PCcarbeneP pincer complexes via water
 elimination from an alcohol proligand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03690F
_journal_year                    2017
_chemical_formula_moiety         'C55 H45 Cl1 Ir1 O1 P3'
_chemical_formula_sum            'C55 H45 Cl Ir O P3'
_chemical_formula_weight         1042.56
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-19
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2017-10-20 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                102.884(2)
_cell_angle_beta                 99.609(2)
_cell_angle_gamma                97.872(2)
_cell_formula_units_Z            4
_cell_length_a                   12.6314(7)
_cell_length_b                   18.2527(12)
_cell_length_c                   21.5647(14)
_cell_measurement_reflns_used    19225
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      26.405
_cell_measurement_theta_min      2.119
_cell_volume                     4699.6(5)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.175
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            85302
_diffrn_reflns_theta_full        26.405
_diffrn_reflns_theta_max         26.405
_diffrn_reflns_theta_min         2.119
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.039
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.067
_platon_squeeze_details
'The largest void volume is sufficient for a maximum of ca. 20 atoms. No solvent molecules could be modelled in this space, and the elemental analysis for compound 7b showed no evidence of solvate molecules.'
_refine_diff_density_max         3.70
_refine_diff_density_min         -4.02
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9423
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         19141
_refine_ls_number_restraints     1255
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.0009856
_refine_ls_shift/su_mean         0.0000163
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1455
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1449
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                12255
_reflns_number_total             19225
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.75
_oxford_diffrn_Wilson_scale      217.85
_oxford_refine_ls_r_factor_ref   0.1153
_oxford_refine_ls_scale          0.069894(10)
_oxford_reflns_number_all        19153
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title CCDC_1568123_Compound_7b
_cod_data_source_file            c7dt03690f2.cif
_cod_data_source_block           Compound7b
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C55 H45 Cl1 Ir1 O1 P3'
_cod_database_code               7044525
_platon_squeeze_void_probe_radius 1.20