Iridium complexes of perimidine-based N-heterocyclic carbene pincer ligands via aminal C-H activation.
Hill, Anthony F.; Ma, Chenxi; McQueen, Caitlin M. A.; Ward, Jas S.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1577–1587; doi:10.1039/c7dt04572g

data_7045211
_publ_section_title
;
 Iridium complexes of perimidine-based N-heterocyclic carbene pincer
 ligands via aminal C-H activation.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1577
_journal_page_last               1587
_journal_paper_doi               10.1039/c7dt04572g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C37 H54 Cl3 Ir1 N2 P2, 2(C6 H6)'
_chemical_formula_sum            'C49 H66 Cl3 Ir N2 P2'
_chemical_formula_weight         1043.60
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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             2016-12-05
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2017-10-11 deposited with the CCDC.
2017-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                98.375(2)
_cell_angle_beta                 94.854(2)
_cell_angle_gamma                100.425(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3051(3)
_cell_length_b                   13.4628(4)
_cell_length_c                   14.1870(3)
_cell_measurement_reflns_used    8831
_cell_measurement_temperature    150
_cell_measurement_theta_max      74
_cell_measurement_theta_min      4
_cell_volume                     2271.87(10)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_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      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15180
_diffrn_reflns_theta_full        67.569
_diffrn_reflns_theta_max         73.834
_diffrn_reflns_theta_min         3.384
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.246
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene'
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.103
_refine_diff_density_max         1.52
_refine_diff_density_min         -1.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8912
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.0009621
_refine_ls_shift/su_mean         0.0000280
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 4.68P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1159
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1159
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                8116
_reflns_number_total             8912
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.77
_oxford_diffrn_Wilson_scale      0.34
_oxford_refine_ls_r_factor_ref   0.0455
_oxford_refine_ls_scale          2.587(19)
_oxford_reflns_number_all        8912
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title
'xcalibur in C:\Users\Kathy\Docu At 20:25 on '
_cod_data_source_file            c7dt04572g2.cif
_cod_data_source_block           KMAb122a
_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 

 Adding full bibliography for 7045206--7045211.cif.
;
_cod_original_cell_volume        2271.87(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C49 H66 Cl3 Ir1 N2 P2'
_cod_database_code               7045211