Intramolecular C-H oxidative addition to iridium(i) triggered by trimethyl phosphite in N,N'-diphosphanesilanediamine complexes.
Passarelli, Vincenzo; Pérez-Torrente, Jesús J; Oro, Luis A.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18596–18606; doi:10.1039/c5dt02886h

data_7036656
_publ_section_title
;
 Intramolecular C-H oxidative addition to iridium(i) triggered by
 trimethyl phosphite in N,N'-diphosphanesilanediamine complexes.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18596
_journal_page_last               18606
_journal_paper_doi               10.1039/c5dt02886h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C46 H58 Ir N2 O6 P4 Si, F6 P, C4 H10 O'
_chemical_formula_sum            'C50 H68 F6 Ir N2 O7 P5 Si'
_chemical_formula_weight         1298.20
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-20 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9408(9)
_cell_length_b                   31.183(2)
_cell_length_c                   14.8638(11)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.110
_cell_measurement_theta_min      2.258
_cell_volume                     5523.8(7)
_computing_cell_refinement       'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_laue_measured_fraction_full 0.986
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            79012
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         1.306
_exptl_absorpt_coefficient_mu    2.654
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.   
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       prism
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.862
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         13146
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+10.0968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10529
_reflns_number_total             13146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02886h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7036656.cif.'
_cod_database_code               7036656
_shelx_estimated_absorpt_t_min   0.503
_shelx_estimated_absorpt_t_max   0.857
_shelxl_version_number           2013-4
_shelx_res_checksum              61894