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_1553190
_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_moiety         'C21 H21 N2 O P Rh, F6 P, C H4 O'
_chemical_formula_sum            'C22 H25 F6 N2 O2 P2 Rh'
_chemical_formula_weight         628.29
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-15 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                83.358(1)
_cell_angle_beta                 74.636(1)
_cell_angle_gamma                74.636(1)
_cell_formula_units_Z            2
_cell_length_a                   9.70447(19)
_cell_length_b                   9.77001(15)
_cell_length_c                   14.1603(3)
_cell_measurement_reflns_used    37776
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      35.00
_cell_measurement_theta_min      2.24
_cell_volume                     1246.84(4)
_computing_cell_refinement       Peaktref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2012/1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41801
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.062
_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     330
_refine_ls_number_reflns         10952
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.5223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0577
_reflns_number_gt                10239
_reflns_number_total             10952
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5qo00287g3.cif
_cod_data_source_block           l0476a
_cod_database_code               1553190