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_7045208
_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 H55 Cl2 Ir1 N2 P2, 2(C6 H6)'
_chemical_formula_sum            'C49 H67 Cl2 Ir N2 P2'
_chemical_formula_weight         1009.16
_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     direct
_audit_update_record
;
2014-03-05 deposited with the CCDC.
2017-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                98.4660(19)
_cell_angle_beta                 94.790(2)
_cell_angle_gamma                100.2717(13)
_cell_formula_units_Z            2
_cell_length_a                   12.3421(4)
_cell_length_b                   13.5109(4)
_cell_length_c                   14.2016(3)
_cell_measurement_reflns_used    47902
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     2290.11(11)
_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 v. 2.01'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.078
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47771
_diffrn_reflns_theta_full        27.542
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_min         2.564
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.137
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.15
_refine_diff_density_min         -1.77
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10547
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.0107133
_refine_ls_shift/su_mean         0.0001319
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 6.37P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1112
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1112
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                8115
_reflns_number_total             10547
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.76
_oxford_diffrn_Wilson_scale      56.13
_oxford_refine_ls_r_factor_ref   0.0792
_oxford_refine_ls_scale          0.15663(6)
_oxford_reflns_number_all        10547
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c7dt04572g2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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.

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
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 -1 '
_cod_original_formula_sum        'C49 H67 Cl2 Ir1 N2 P2'
_cod_database_code               7045208
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT H(1,X'S) UNTIL H(3) 
REM CONT CL(2,OCC), CL(3,OCC), CL(1,OCC) 
REM SUMFIX CL(1,OCC) UNTIL CL(3) 
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   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) H   ( 642,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
U(IJ) 0.0, 0.1 = C(81) TO C(82) 
U(IJ) 0.0, 0.1 = C(82) TO C(83) 
U(IJ) 0.0, 0.1 = C(83) TO C(84) 
U(IJ) 0.0, 0.1 = C(84) TO C(85) 
U(IJ) 0.0, 0.1 = C(85) TO C(86) 
U(IJ) 0.0, 0.1 = C(86) TO C(81) 
DIST 1.39, 0.01 = C(81) TO C(82), C(82) TO C(83), C(83) TO C(84) 
DIST 1.39, 0.01 = C(84) TO C(85), C(85) TO C(86), C(86) TO C(81) 
ANGLE 0.0, 0.1 = MEAN P(1) TO IR(1) TO H(2), P(1) TO IR(1) TO CL(2) 
ANGLE 0.0, 0.1 = MEAN C(1) TO IR(1) TO H(2), C(1) TO IR(1) TO CL(2) 
DIST 1.5, 0.02 = IR(1) TO H(2) 
ANGLE 0.0, 0.1 = MEAN P(1) TO IR(1) TO H(3), P(1) TO IR(1) TO CL(3) 
ANGLE 0.0, 0.1 = MEAN C(1) TO IR(1) TO H(3), C(1) TO IR(1) TO CL(3) 
DIST 1.5, 0.02 = IR(1) TO H(3) 
ANGLE 0.0, 0.1 = MEAN P(1) TO IR(1) TO H(1), P(1) TO IR(1) TO CL(1) 
ANGLE 0.0, 0.1 = MEAN C(1) TO IR(1) TO H(1), C(1) TO IR(1) TO CL(1) 
DIST 1.5, 0.02 = IR(1) TO H(1) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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