Chemoselective synthesis of heterobimetallic bis-NHC complexes.
Dutschke, Patrick D.; Bente, Stefanie; Daniliuc, Constantin G.; Kinas, Jenny; Hepp, Alexander; Hahn, F. Ekkehardt; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14388–14392; doi:10.1039/d0dt03369c

data_7705647
_publ_section_title
;
 Chemoselective synthesis of heterobimetallic bis-NHC complexes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14388
_journal_page_last               14392
_journal_paper_doi               10.1039/d0dt03369c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C29 H33 I2 Ir N6 O2, 2(C2 H3 N)'
_chemical_formula_sum            'C33 H39 I2 Ir N8 O2'
_chemical_formula_weight         1025.72
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-05 deposited with the CCDC.	2020-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                116.8130(10)
_cell_angle_beta                 105.4610(10)
_cell_angle_gamma                91.0970(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4757(2)
_cell_length_b                   15.2789(3)
_cell_length_c                   15.8657(3)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.10
_cell_measurement_theta_min      2.67
_cell_volume                     1743.98(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.902
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33039
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.303
_diffrn_reflns_theta_min         1.512
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.641
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.4897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1281 before and 0.0403 after correction. The Ratio of minimum to maximum transmission is 0.6561. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.512
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         11192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.2400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10273
_reflns_number_total             11192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03369c2.cif
_cod_data_source_block           pd1
_cod_depositor_comments
'Adding full bibliography for 7705647--7705651.cif.'
_cod_original_cell_volume        1743.98(6)
_cod_database_code               7705647
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.646
_shelx_estimated_absorpt_t_min   0.342
_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.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C16(H16), C21(H21), C22(H22)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C38(H38A,H38B,H38C), C36(H36A,H36B,H36C)
;
_olex2_date_sample_data_collection 2019-09-09
_olex2_date_sample_submission    2019-09-09
_olex2_submission_original_sample_id pd190909
_olex2_submission_special_instructions 'No special instructions were received'