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_4517817
_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            'C50 H42 Br2 Cl13 Ir N10 P2'
_chemical_formula_weight         1657.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 95.9080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4686(5)
_cell_length_b                   18.0388(8)
_cell_length_c                   31.6485(13)
_cell_measurement_reflns_used    9640
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.210
_cell_measurement_theta_min      2.293
_cell_volume                     5944.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            110068
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.423
_diffrn_reflns_theta_min         3.427
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    4.275
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.5336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.574
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         22578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+11.9589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17522
_reflns_number_total             22578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02290_si_006.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4517817
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.280
_shelx_estimated_absorpt_t_max   0.482
_shelx_res_checksum              63254
_shelx_hkl_checksum              37564