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_7044524
_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         'C87 H73 B1 F24 Ir1 P3'
_chemical_formula_sum            'C87 H73 B F24 Ir P3'
_chemical_formula_weight         1870.45
_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     other
_audit_creation_date             2017-09-23
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_audit_update_record
;
2017-10-20 deposited with the CCDC.
2017-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                104.677(3)
_cell_angle_beta                 100.375(3)
_cell_angle_gamma                95.711(3)
_cell_formula_units_Z            4
_cell_length_a                   20.144(2)
_cell_length_b                   20.626(2)
_cell_length_c                   21.132(3)
_cell_measurement_reflns_used    33867
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.460
_cell_measurement_theta_min      2.133
_cell_volume                     8257.0(16)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.126
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            119120
_diffrn_reflns_theta_full        25.931
_diffrn_reflns_theta_max         26.460
_diffrn_reflns_theta_min         2.133
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3752
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.144
_platon_squeeze_details
'The largest void volume is sufficient for a maximum of ca. 14 atoms. No solvent molecules could be modelled in this space, and the elemental analysis for compound 4 showed no evidence of solvate molecules.'
_refine_diff_density_max         5.47
_refine_diff_density_min         -3.93
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0259
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2170
_refine_ls_number_reflns         33702
_refine_ls_number_restraints     2487
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.0035759
_refine_ls_shift/su_mean         0.0000293
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1812
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1801
_reflns_limit_h_max              24
_reflns_limit_h_min              -25
_reflns_limit_k_max              24
_reflns_limit_k_min              -25
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                21251
_reflns_number_total             33867
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.35
_oxford_diffrn_Wilson_scale      867.39
_oxford_refine_ls_r_factor_ref   0.1240
_oxford_refine_ls_scale          0.036742(3)
_oxford_reflns_number_all        33744
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title CCDC_1568125_Compound_4
_cod_data_source_file            c7dt03690f2.cif
_cod_data_source_block           Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        8257.0(17)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C87 H73 B1 F24 Ir1 P3'
_cod_database_code               7044524
_platon_squeeze_void_probe_radius 1.20