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_4517819
_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_sum            'C49 H51 Cl Fe I Ir N4 O4 P2'
_chemical_formula_weight         1232.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.113(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2092(8)
_cell_length_b                   11.5302(14)
_cell_length_c                   28.4666(15)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.75
_cell_measurement_theta_min      2.27
_cell_volume                     4660.7(7)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            86361
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.257
_diffrn_reflns_theta_min         1.906
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    4.001
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5058
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       prism
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.343
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         15416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+1.3299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13179
_reflns_number_total             15416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02290_si_005.cif
_cod_data_source_block           new
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4517819
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.456
_shelx_estimated_absorpt_t_max   0.751
_shelx_res_checksum              52022
_shelx_hkl_checksum              3127