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_7044521
_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_absolute_configuration unk
_chemical_formula_moiety         'C37 H28 Cl1 Ir1 P2'
_chemical_formula_sum            'C37 H28 Cl Ir P2'
_chemical_formula_weight         762.25
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2017-10-18
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.741(2)
_cell_length_b                   18.6304(11)
_cell_length_c                   9.7858(6)
_cell_measurement_reflns_used    27124
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.463
_cell_measurement_theta_min      2.432
_cell_volume                     5969.1(6)
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.035
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            27124
_diffrn_reflns_theta_full        26.463
_diffrn_reflns_theta_max         26.463
_diffrn_reflns_theta_min         2.432
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.696
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.46
_refine_ls_abs_structure_details 'Flack (1983), 1385 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.036(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0037
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3007
_refine_ls_number_restraints     214
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.0023450
_refine_ls_shift/su_mean         0.0001074
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +21.90P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0678
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0678
_reflns_limit_h_max              40
_reflns_limit_h_min              0
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              -12
_reflns_number_gt                2818
_reflns_number_total             3018
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0264
_oxford_refine_ls_scale          0.027131(2)
_oxford_reflns_number_all        3007
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title CCDC_1568120_Compound_2
_cod_data_source_file            c7dt03690f2.cif
_cod_data_source_block           Compound2
_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_sg_symbol_H-M      'F d d 2 '
_cod_original_formula_sum        'C37 H28 Cl1 Ir1 P2'
_cod_database_code               7044521
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S  U'S 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
LIMIT      0.01000000 U[ISO] 
LIMIT      0.01000000 X 
LIMIT      0.01000000 Y 
LIMIT      0.01000000 Z 
LIMIT      0.01000000 U[11] 
LIMIT      0.01000000 U[22] 
LIMIT      0.01000000 U[33] 
LIMIT      0.01000000 U[12] 
LIMIT      0.01000000 U[13] 
LIMIT      0.01000000 U[23] 
LIMIT      0.01000000 OCC 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = CL(1) TO C(1) 
VIBRATION 0.0, 0.020000 = CL(1) TO C(1) 
END                                                                             
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