Bypassing the lack of reactivity of endo-substituted norbornenes with the catalytic rectification–insertion mechanism
Commarieu, Basile; Claverie, Jerome P.; Chem. Sci. 6 (2015) 2172–; doi:10.1039/C4SC03575E

data_1518478
_publ_section_title
;
 Bypassing the lack of reactivity of endo-substituted norbornenes with the
 catalytic rectification--insertion mechanism
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2172
_journal_paper_doi               10.1039/C4SC03575E
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C22 H35 F6 O6 Pd Sb'
_chemical_formula_weight         737.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-11-17 deposited with the CCDC.
2014-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.758(3)
_cell_length_b                   16.947(4)
_cell_length_c                   9.5046(19)
_cell_measurement_reflns_used    3837
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.40
_cell_volume                     2699.3(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17478
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.809
_diffrn_reflns_theta_min         1.709
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
; 
 Flack x determined using 2133 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.031(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6048
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0222P)^2^+1.3018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.892
_reflns_number_gt                5361
_reflns_number_total             6048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03575e2.cif
_cod_data_source_block           clav010a
_cod_depositor_comments
'Adding full bibliography for 1518476--1518480.cif.'
_cod_database_code               1518478
_shelx_estimated_absorpt_t_min   0.527
_shelx_estimated_absorpt_t_max   0.819
_shelxl_version_number           2013-3
_shelx_res_checksum              52539
_shelx_hkl_checksum              28670