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_4517815
_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         'C41 H35 Cl2 Fe Ir N4 O2 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C49 H51 Cl2 Fe Ir N4 O4 P2'
_chemical_formula_weight         1140.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                104.650(2)
_cell_angle_beta                 107.734(2)
_cell_angle_gamma                95.338(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7350(3)
_cell_length_b                   12.2363(3)
_cell_length_c                   17.4937(5)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.30
_cell_volume                     2275.06(11)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0508
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31619
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.980
_diffrn_reflns_theta_min         1.750
_exptl_absorpt_coefficient_mu    3.479
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5711
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.361
_refine_diff_density_min         -1.845
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         10922
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+19.4284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9806
_reflns_number_total             10922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02290_si_004.cif
_cod_data_source_block           sad_a
_cod_database_code               4517815
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.412
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.04
3.a Ternary CH refined with riding coordinates:
 C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45)
3.b Secondary CH2 refined with riding coordinates:
 C101(H10D,H10E), C102(H10F,H10G), C103(H10H,H10I), C104(H10J,H10K), C201(H20A,
 H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              75526
_shelx_hkl_checksum              79761
_olex2_submission_special_instructions 'No special instructions were received'