Acetals from Primary Alcohols with the Use of Tridentate Proton Responsive Phosphinepyridonate Iridium Catalysts
Sahoo, Apurba Ranjan; Jiang, Fan; Bruneau, Christian; Sharma, Gangavaram VM; Suresh, Surisetti; Achard, Mathieu; RSC Adv.  (2016) –; doi:10.1039/C6RA23946C

data_7226800
_publ_section_title
;
 Acetals from Primary Alcohols with the Use of Tridentate Proton
 Responsive Phosphinepyridonate Iridium Catalysts
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA23946C
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H32 Cl Ir N2 O2 P, Cl'
_chemical_formula_sum            'C28 H32 Cl2 Ir N2 O2 P'
_chemical_formula_weight         722.62
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.093(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.484(4)
_cell_length_b                   8.4074(8)
_cell_length_c                   21.803(2)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.22
_cell_measurement_wavelength     0.71073
_cell_volume                     6720.6(11)
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2014)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.941
_exptl_absorpt_coefficient_mu    4.203
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       prism
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.090
_refine_diff_density_max         4.826
_refine_diff_density_min         -3.417
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         7665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1543P)^2^+123.1515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2702
_refine_ls_wR_factor_ref         0.2959
_reflns_number_gt                5452
_reflns_number_total             7665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra23946c2.cif
_cod_data_source_block           MAARS714
_cod_original_cell_volume        6720.7(12)
_cod_database_code               7226800
_shelx_res_checksum              91719