Four Consecutive Reactions in one Pot: Cascade Formation of an Unprecedented Triphosphatricyclo[3.2.1.02,7]oct-3-ene
Giese, Steven; Buzsaki, Daniel; Nyulaszi, Laszlo; Muller, Christian; Chemical Communications  (2019) –; doi:10.1039/C9CC07462G

data_7124291
_publ_section_title
;
 Four Consecutive Reactions in one Pot: Cascade Formation of an
 Unprecedented Triphosphatricyclo[3.2.1.02,7]oct-3-ene
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07462G
_journal_year                    2019
_chemical_formula_moiety         '(Au 1+)1, (C21 H33 O2 P3 Si3)1, (Cl)1'
_chemical_formula_sum            'C21 H33 Au Cl O2 P3 Si3'
_chemical_formula_weight         727.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.741(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2862(18)
_cell_length_b                   11.6119(14)
_cell_length_c                   19.290(3)
_cell_measurement_reflns_used    9691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.44
_cell_volume                     2941.5(7)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0705
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            91626
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.431
_diffrn_reflns_theta_min         2.341
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.394
_exptl_absorpt_correction_T_max  0.4130
_exptl_absorpt_correction_T_min  0.2866
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-Pentane'
_exptl_crystal_size_max          0.280
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_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.498
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.090
_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_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0169
_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^)+(0.0173P)^2^+1.9870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                5668
_reflns_number_total             6044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07462g2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2941.4(7)
_cod_database_code               7124291
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.314
_shelx_estimated_absorpt_t_max   0.519
_shelx_res_checksum              81089