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_4517816
_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 Cl I Ir N4 O2 P2, 2(C H Cl3)'
_chemical_formula_sum            'C45 H39 Cl7 I Ir N4 O2 P2'
_chemical_formula_weight         1297.073
_chemical_name_systematic        IrHCl(TheophyllineI_kO1_kN7_(PPh3)2]_x2CHCl3
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-02
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.227(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6487(2)
_cell_length_b                   19.0356(3)
_cell_length_c                   18.3707(3)
_cell_measurement_reflns_used    9127
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      55.185
_cell_measurement_theta_min      4.948
_cell_volume                     4744.75(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.9994
_diffrn_reflns_Laue_measured_fraction_max 0.9971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            68983
_diffrn_reflns_point_group_measured_fraction_full 0.9994
_diffrn_reflns_point_group_measured_fraction_max 0.9971
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         1.84
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.969
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Multi-scan correction included in APEX2 package (Bruker AXS, 2012)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       colourless
_exptl_crystal_F_000             2528.360
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.192
_refine_diff_density_max         3.1925
_refine_diff_density_min         -2.7075
_refine_diff_density_rms         0.1936
_refine_ls_d_res_high            0.7669
_refine_ls_d_res_low             11.0487
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0374
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     566
_refine_ls_number_reflns         10990
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.0365
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+37.0705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                10228
_reflns_number_total             10990
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ao0c02290_si_003.cif
_cod_data_source_block           jb170410_0m
_cod_database_code               4517816
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.516
_shelx_estimated_absorpt_t_min   0.324
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Cl7, Cl2, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Cl7 \\sim Cl2 \\sim Cl4: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(Cl7) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
4.a Ternary CH refined with riding coordinates:
 C48(H48), C49(H49)
4.b 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), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47)
4.c Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c)
;
_olex2_submission_special_instructions 'No special instructions were received'