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_7045210
_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_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C57 H62 Cl4 Ir2 N2 P2, C1 H1 Cl3'
_chemical_formula_sum            'C58 H63 Cl7 Ir2 N2 P2'
_chemical_formula_weight         1482.71
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             14-04-08
_audit_creation_method           CRYSTALS_ver_14.23
_audit_update_record
;
2017-10-11 deposited with the CCDC.
2017-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9066(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2252(2)
_cell_length_b                   23.9867(4)
_cell_length_c                   15.3547(2)
_cell_measurement_reflns_used    74484
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.55
_cell_volume                     5604.47(14)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for windows (Farrugia, 1997)'
_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      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.091
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            86883
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.560
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.175
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             2912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform/pentane'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.33
_refine_diff_density_min         -1.83
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9639
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9863
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.0037541
_refine_ls_shift/su_mean         0.0000781
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 10.8 15.7 7.82 2.19 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1272
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1272
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7367
_reflns_number_total             9877
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.27
_oxford_diffrn_Wilson_scale      214.43
_oxford_refine_ls_r_factor_ref   0.0692
_oxford_refine_ls_scale          0.070052(13)
_oxford_reflns_number_all        9863
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMA011 At 14:51 on 8/ 4'
_cod_data_source_file            c7dt04572g2.cif
_cod_data_source_block           CMA011
_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_sg_symbol_H-M      'P 21/a '
_cod_database_code               7045210
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, U'S 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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