Transforming a chemically labile [2+3] imine cage into a robust carbamate cage
Mastalerz, Michael; Hu, Xin-Yue; Zhang, Wen-Shan; Schröder, Rasmus R.; Wacker, Irene; Rominger, Frank -; Chem. Commun.  (2017) –; doi:10.1039/C7CC03677A

data_7120397
_publ_section_title
;
 Transforming a chemically labile [2+3] imine cage into a robust carbamate
 cage
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03677A
_journal_year                    2017
_chemical_formula_sum            'C88 H52 N6 O12'
_chemical_formula_weight         1385.35
_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-2014/7
_audit_update_record
;
2017-05-02 deposited with the CCDC.
2017-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                76.070(2)
_cell_angle_beta                 87.338(2)
_cell_angle_gamma                84.030(2)
_cell_formula_units_Z            4
_cell_length_a                   18.7671(3)
_cell_length_b                   19.4091(4)
_cell_length_c                   27.7570(6)
_cell_measurement_reflns_used    86976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.00
_cell_measurement_theta_min      2.36
_cell_volume                     9757.6(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'STOE Stadivari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
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_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.630
_diffrn_reflns_theta_min         2.356
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  1.692
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_description       needle
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.363
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_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         34263
_refine_ls_number_restraints     5643
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_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+14.4856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25908
_reflns_number_total             34263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03677a2.cif
_cod_data_source_block           xh1_sq
_cod_database_code               7120397
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.975
_exptl_absorpt_special_details   'STOE X-AREA Laue Analyzer'
_shelx_res_checksum              93518
_shelx_fab_checksum              21090