Irida-β-ketoimines Derived from Hydrazines To Afford Metallapyrazoles or N-N Bond Cleavage: A Missing Metallacycle Disclosed by a Theoretical and Experimental Study.
Zumeta, Itziar; Mendicute-Fierro, Claudio; Bustos, Itxaso; Huertos, Miguel A.; Rodríguez-Diéguez, Antonio; Seco, José M; San Sebastian, Eider; Garralda, María A; Inorganic chemistry 55 (2016) 10284–10293; doi:10.1021/acs.inorgchem.6b01550

data_4348741
_publ_section_title
;
 Irida-\b-ketoimines Derived from Hydrazines To Afford Metallapyrazoles or
 N-N Bond Cleavage: A Missing Metallacycle Disclosed by a Theoretical and
 Experimental Study.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10284
_journal_page_last               10293
_journal_paper_doi               10.1021/acs.inorgchem.6b01550
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C43 H38 Cl10 Ir N O2 P2'
_chemical_formula_weight         1209.38
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
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_cell_length_b                   39.188(3)
_cell_length_c                   12.8242(11)
_cell_measurement_reflns_used    12488
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.52
_cell_measurement_theta_min      2.23
_cell_volume                     19694(3)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker ApexII'
_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 0.798
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.798
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            81044
_diffrn_reflns_point_group_measured_fraction_full 0.798
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.335
_diffrn_reflns_theta_min         1.470
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.356
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             9536
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7119
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+52.1776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6099
_reflns_number_total             7119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01550_si_001.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        19694(4)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4348741
_shelxl_version_number           2014-3
_shelx_res_checksum              85494
_shelx_hkl_checksum              32833