Acyl(furfurylamine)iridium(III) complexes from irida-β-diketones. Characterisation and catalytic activity in amine-borane hydrolysis
Bustos, Itxaso; Seco, Jose M.; Rodríguez-Diéguez, Antonio; Garralda, María A.; Mendicute-Fierro, Claudio; Inorganica Chimica Acta 498 (2019) 119165–; doi:10.1016/j.ica.2019.119165

data_1565809
_publ_section_title
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 Acyl(furfurylamine)iridium(III) complexes from irida-\b-diketones.
 Characterisation and catalytic activity in amine-borane hydrolysis
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_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119165
_journal_paper_doi               10.1016/j.ica.2019.119165
_journal_volume                  498
_journal_year                    2019
_chemical_formula_sum            'C44 H39 Cl Ir N O4 P2'
_chemical_formula_weight         935.35
_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_method           SHELXL-2014
_cell_angle_alpha                93.039(4)
_cell_angle_beta                 104.688(4)
_cell_angle_gamma                105.298(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4310(12)
_cell_length_b                   10.5830(17)
_cell_length_c                   18.558(2)
_cell_measurement_reflns_used    55841
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      2.57
_cell_volume                     1895.6(4)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            91216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.771
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.722
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0706 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.9433.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             932
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0171
_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^)+(0.0134P)^2^+1.2688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0407
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9252
_reflns_number_total             9857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119165.cif
_cod_data_source_block           Compound3
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
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_cod_database_code               1565809
_shelxl_version_number           2014-3