Formation of exceptionally weak C‒C bonds by metal-templated pinacol coupling
Folkertsma, E.; Benthem, S. H.; Witteman, L.; van Slagmaat, C. A. M. R.; Lutz, M.; Klein Gebbink, R. J. M.; Moret, M.-E.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01130J

data_7042814
_publ_section_title
;
 Formation of exceptionally weak C--C bonds by metal-templated pinacol
 coupling
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01130J
_journal_year                    2017
_chemical_formula_moiety         'C66 H52 Cl2 N8 O2 Zn2'
_chemical_formula_sum            'C66 H52 Cl2 N8 O2 Zn2'
_chemical_formula_weight         1190.79
_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
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-24 deposited with the CCDC.
2017-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                67.700(2)
_cell_angle_beta                 72.709(2)
_cell_angle_gamma                79.513(2)
_cell_formula_units_Z            1
_cell_length_a                   10.6545(4)
_cell_length_b                   12.7083(6)
_cell_length_c                   15.0735(6)
_cell_measurement_reflns_used    26629
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.49
_cell_volume                     1797.43(13)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31525
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.508
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       block
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8256
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0375P)^2^+0.5777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7375
_reflns_number_total             8256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01130j2.cif
_cod_data_source_block           l0771g
_cod_original_cell_volume        1797.44(14)
_cod_database_code               7042814
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              86765
_shelx_fab_checksum              22534