Rhodium catalysed conversion of carbenes into ketenes and ketene imines using PNN pincer complexes
Tang, Z.; Mandal, S.; Paul, N. D.; Lutz, M.; Li, P.; van der Vlugt, J. I.; de Bruin, B.; Organic Chemistry Frontiers 2 (2015) 1561–; doi:10.1039/C5QO00287G

data_1553189
_publ_section_title
;
 Rhodium catalysed conversion of carbenes into ketenes and ketene imines
 using PNN pincer complexes
;
_journal_issue                   12
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1561
_journal_paper_doi               10.1039/C5QO00287G
_journal_volume                  2
_journal_year                    2015
_chemical_formula_sum            'C20 H27 F6 N2 O P2 Rh'
_chemical_formula_weight         590.28
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-11 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.462(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4021(9)
_cell_length_b                   10.9937(7)
_cell_length_c                   15.6906(10)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.6204
_cell_measurement_theta_min      4.8606
_cell_volume                     2292.3(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker ApexII Triumph monochromator sealed tube'
_diffrn_measurement_method       'Photon 50 CMOS detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            97401
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.480
_diffrn_reflns_theta_min         3.406
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.5796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'translucent intense yellow-brown'
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.886
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.631
_refine_diff_density_min         -2.366
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         14600
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+1.5557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10763
_reflns_number_total             14600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qo00287g3.cif
_cod_data_source_block           TZ814_0m_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1553189
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              30547
_shelx_hkl_checksum              68807