Selective synthesis of iridium(iii) end-capped polyynes by oxidative addition of 1-iodopolyynes to Vaska's complex.
Pigulski, Bartłomiej; Jarszak, Agata; Szafert, Sławomir; Dalton transactions (Cambridge, England : 2003) 47 (2018) 17046–17054; doi:10.1039/c8dt04219e

data_7048005
_publ_section_title
;
 Selective synthesis of iridium(iii) end-capped polyynes by oxidative
 addition of 1-iodopolyynes to Vaska's complex.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17046
_journal_page_last               17054
_journal_paper_doi               10.1039/c8dt04219e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C47 H34 Cl I Ir N O3 P2, C7 H8'
_chemical_formula_sum            'C54 H42 Cl I Ir N O3 P2'
_chemical_formula_weight         1169.37
_chemical_name_systematic
Carbonyl(chloro)iodo[4-(4-nitrophenyl)butadiynyl]bis(triphenylphosphine)iridium(III)
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-04-27 deposited with the CCDC.
2018-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.8141
_cell_measurement_theta_min      2.9354
_cell_volume                     4642(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
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_diffrn_measurement_device_type  'KUMA KM-4 CCD'
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.3488
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.552
_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_l_min       -32
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_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.552
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         36.901
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.714
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.673
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_exptl_crystal_size_mid          0.060
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_refine_diff_density_max         1.619
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         12946
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      0.763
_refine_ls_R_factor_all          0.1792
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0325P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5253
_reflns_number_total             12946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04219e2.cif
_cod_data_source_block           2-C4[Ir]I
_cod_depositor_comments          'Adding full bibliography for 7048005.cif.'
_cod_database_code               7048005
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.571
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_shelx_res_checksum              19526