Synthesis of IrIII Hydrido Complexes by Oxidative Addition of Halogenated Theophylline and Adenine Derivatives
Blumenberg, Jonas; Kampert, Florian; Hepp, Alexander; Hahn, F. Ekkehardt; ACS Omega  (2020) –; doi:10.1021/acsomega.0c02290

data_4517818
_publ_section_title
;
 Synthesis of IrIII Hydrido Complexes by Oxidative Addition of Halogenated
 Theophylline and Adenine Derivatives
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.0c02290
_journal_year                    2020
_chemical_formula_moiety
'C43 H37 N4 O2 P2 Cl2 Ir, 1.2(C7 H8), 0.3 (C6 H6)'
_chemical_formula_sum            'C53.2 H48.8 Cl2 Ir N4 O2 P2'
_chemical_formula_weight         1101.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.8550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.4221(9)
_cell_length_b                   18.4724(5)
_cell_length_c                   18.3313(6)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.6215
_cell_measurement_theta_min      3.2305
_cell_volume                     10564.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85631
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.711
_diffrn_reflns_theta_min         2.613
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.731
_exptl_absorpt_correction_T_max  0.7051
_exptl_absorpt_correction_T_min  0.5707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Multi-scan correction included in APEX3 package (Bruker AXS, 2014)
 
 87844 Corrected reflections used
 Estimated minimum and maximum transmission:  0.5707  0.7051
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.2390
 Lambda/2 correction factor = 0.00150
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       plate
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.577
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         12313
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+77.3554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10710
_reflns_number_total             12313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02290_si_002.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C53.20 H48.80 Cl2 Ir N4 O2 P2'
_cod_database_code               4517818
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              61766
_shelx_hkl_checksum              69738