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_1518480
_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_moiety         'C56 H76 O16 Pd4, 4(F6 Sb), 5(C2 H2 Cl4)'
_chemical_formula_sum            'C66 H86 Cl20 F24 O16 Pd4 Sb4'
_chemical_formula_weight         3212.94
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                66.181(2)
_cell_angle_beta                 88.434(2)
_cell_angle_gamma                72.775(2)
_cell_formula_units_Z            2
_cell_length_a                   16.4284(14)
_cell_length_b                   19.3745(17)
_cell_length_c                   21.4447(19)
_cell_measurement_reflns_used    8466
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.27
_cell_measurement_theta_min      2.20
_cell_volume                     5930.9(9)
_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 0.989
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79047
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         1.585
_exptl_absorpt_coefficient_mu    2.025
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       block
_exptl_crystal_F_000             3108
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.088
_platon_squeeze_details
;
PLATON Reference : 
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
Spek, A.L. (2009). Acta Cryst. D65, 148-155.

Void space analysis consistent with
a fifth, severely disordered C2CH2Cl4 molecule
of solvation.
;
_refine_diff_density_max         1.980
_refine_diff_density_min         -1.241
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_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0629P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15699
_reflns_number_total             27085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03575e2.cif
_cod_data_source_block           clav008s-sr
_cod_depositor_comments
'Adding full bibliography for 1518476--1518480.cif.'
_cod_database_code               1518480
_shelx_estimated_absorpt_t_min   0.709
_shelx_estimated_absorpt_t_max   0.842
_shelxl_version_number           2013-2
_shelx_res_checksum              88753
_shelx_hkl_checksum              93137