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_7045209
_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         'C37 H30 Cl1 Ir1 N2 P2, C7 H8'
_chemical_formula_sum            'C44 H38 Cl Ir N2 P2'
_chemical_formula_weight         884.42
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             14-09-29
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2014-12-17 deposited with the CCDC.
2017-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.0755(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1881(3)
_cell_length_b                   13.2047(2)
_cell_length_c                   21.6283(3)
_cell_measurement_reflns_used    10677
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     3737.78(12)
_computing_cell_refinement       'CrysAlis PRO, (Agilent Technologies, 2013)'
_computing_data_collection       'Supernova, (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlis PRO, (Agilent Technologies, 2013)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23422
_diffrn_reflns_theta_full        68.390
_diffrn_reflns_theta_max         72.175
_diffrn_reflns_theta_min         3.930
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.639
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.37
_refine_diff_density_min         -1.41
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9862
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7245
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.0011493
_refine_ls_shift/su_mean         0.0000235
_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: 
 0.271E+04 0.442E+04 0.286E+04 0.129E+04 334. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1339
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1338
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6158
_reflns_number_total             7277
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.93
_oxford_diffrn_Wilson_scale      0.26
_oxford_refine_ls_r_factor_ref   0.0552
_oxford_refine_ls_scale          2.179(15)
_oxford_reflns_number_all        7247
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'C:\Users\Hill Group\Desktop\Jas At 14:39 on '
_cod_data_source_file            c7dt04572g2.cif
_cod_data_source_block           CMA005f(OB)
_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/c '
_cod_original_formula_sum        'C44 H38 Cl1 Ir1 N2 P2'
_cod_database_code               7045209
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.02 = C(101) TO C(102) 
U(IJ) 0.0, 0.02 = C(102) TO C(103) 
U(IJ) 0.0, 0.02 = C(103) TO C(104) 
U(IJ) 0.0, 0.02 = C(104) TO C(105) 
U(IJ) 0.0, 0.02 = C(105) TO C(106) 
U(IJ) 0.0, 0.02 = C(106) TO C(107) 
U(IJ) 0.0, 0.02 = C(107) TO C(101) 
REM 
DIST 0.0, 0.01 = MEAN C(101) TO C(102), C(102) TO C(103) 
DIST 0.0, 0.01 = MEAN C(102) TO C(103), C(103) TO C(104) 
DIST 0.0, 0.01 = MEAN C(103) TO C(104), C(104) TO C(105) 
DIST 0.0, 0.01 = MEAN C(104) TO C(105), C(105) TO C(106) 
DIST 0.0, 0.01 = MEAN C(105) TO C(106), C(106) TO C(101) 
DIST 0.0, 0.01 = MEAN C(106) TO C(101), C(101) TO C(102) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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