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_1553188
_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            'C26 H23 F6 N2 O P2 Rh'
_chemical_formula_weight         658.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 100.416(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6439(13)
_cell_length_b                   11.6245(14)
_cell_length_c                   21.782(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2650.7(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0711
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30389
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.903
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.319
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4661
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+5.0183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3905
_reflns_number_total             4661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qo00287g3.cif
_cod_data_source_block           TZ888_2_0m_a
_cod_original_cell_volume        2650.7(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1553188
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.738
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              20373
_shelx_hkl_checksum              18093