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_7045207
_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 N2 P2 Rh2, C1 H1 Cl3'
_chemical_formula_sum            'C58 H63 Cl7 N2 P2 Rh2'
_chemical_formula_weight         1304.08
_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             14-03-15
_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                 91.8919(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2362(2)
_cell_length_b                   23.9600(3)
_cell_length_c                   15.33320(10)
_cell_measurement_reflns_used    184256
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     5594.48(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 (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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.049
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            115477
_diffrn_reflns_theta_full        27.474
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         2.562
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.022
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_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform/pentane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.57
_refine_diff_density_min         -1.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9789
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         12795
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.0044362
_refine_ls_shift/su_mean         0.0001437
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +15.27P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1438
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1438
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                9781
_reflns_number_total             12798
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.25
_oxford_diffrn_Wilson_scale      34.90
_oxford_refine_ls_r_factor_ref   0.0698
_oxford_refine_ls_scale          0.19472(10)
_oxford_reflns_number_all        12795
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMA001 At 12:50 on 15/ 3'
_cod_data_source_file            c7dt04572g2.cif
_cod_data_source_block           CMA001
_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               7045207
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;