Intermolecular C-H activation with an Ir-METAMORPhos piano-stool complex - multiple reaction steps at a reactive ligand.
Oldenhof, S.; Lutz, M.; van der Vlugt, J. I.; Reek, J. N. H.; Chemical communications (Cambridge, England) 51 (2015) 15200–15203; doi:10.1039/c5cc05916j

data_7117876
_publ_section_title
;
 Intermolecular C-H activation with an Ir-METAMORPhos piano-stool complex
 - multiple reaction steps at a reactive ligand.
;
_journal_issue                   82
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15200
_journal_page_last               15203
_journal_paper_doi               10.1039/c5cc05916j
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C32 H38 Cl Ir N O2 P S'
_chemical_formula_sum            'C32 H38 Cl Ir N O2 P S'
_chemical_formula_weight         759.31
_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   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-06 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.9132(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3385(17)
_cell_length_b                   14.6511(17)
_cell_length_c                   15.2223(18)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.20
_cell_volume                     3042.8(6)
_computing_cell_refinement       'SAINT V8.27B'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V8.27B, SADABS-2012/1'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'coordinates from Rh complex'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0127
_diffrn_reflns_av_unetI/netI     0.0079
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45334
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         1.707
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.627
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.2755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0126
_refine_ls_R_factor_gt           0.0118
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+2.1251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0293
_refine_ls_wR_factor_ref         0.0296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6806
_reflns_number_total             7021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05916j2.cif
_cod_data_source_block           l0548a
_cod_database_code               7117876
_shelxl_version_number           2013-3
_shelx_res_checksum              16031