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_7044526
_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         'C105.50 H71 B1 Cl1 F24 Ir1 P4'
_chemical_formula_sum            'C105.5 H71 B Cl F24 Ir P4'
_chemical_formula_weight         2157.06
_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             2017-10-23
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2017-10-23 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                73.9920(15)
_cell_angle_beta                 74.3769(18)
_cell_angle_gamma                83.4459(16)
_cell_formula_units_Z            2
_cell_length_a                   12.7542(6)
_cell_length_b                   17.2595(7)
_cell_length_c                   22.2988(10)
_cell_measurement_reflns_used    18591
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      26.413
_cell_measurement_theta_min      2.128
_cell_volume                     4539.8(4)
_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  0.062
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            82853
_diffrn_reflns_theta_full        26.413
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         2.128
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.670
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       wedge
_exptl_crystal_F_000             2158
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.57
_refine_diff_density_min         -2.13
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9832
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         18521
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.0041084
_refine_ls_shift/su_mean         0.0000622
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +19.19P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0862
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0861
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              21
_reflns_limit_k_min              -20
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                16063
_reflns_number_total             18591
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.71
_oxford_diffrn_Wilson_scale      164.54
_oxford_refine_ls_r_factor_ref   0.0489
_oxford_refine_ls_scale          0.082063(9)
_oxford_reflns_number_all        18523
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title CCDC_1568121_Compound_5
_cod_data_source_file            c7dt03690f2.cif
_cod_data_source_block           Compound5
_cod_original_cell_volume        4539.8(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C105.50 H71 B1 Cl1 F24 Ir1 P4'
_cod_database_code               7044526