[6]Saddlequat: a [6]helquat captured on its racemization pathway
Adriaenssens, Louis; Severa, Lukáš; Koval, Dušan; Císařová, Ivana; Belmonte, Marta Martínez; Escudero-Adán, Eduardo C.; Novotná, Pavlína; Sázelová, Petra; Vávra, Jan; Pohl, Radek; Šaman, David; Urbanová, Marie; Kašička, Václav; Teplý, Filip; Chemical Science 2 (2011) 2314–; doi:10.1039/c1sc00468a

data_1515533
_publ_section_title
;
 [6]Saddlequat: a [6]helquat captured on its racemization pathway
;
_journal_issue                   12
_journal_name_full               'Chemical Science'
_journal_page_first              2314
_journal_paper_doi               10.1039/c1sc00468a
_journal_volume                  2
_journal_year                    2011
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C27 H26 N2, 2(F6 P)'
_chemical_formula_sum            'C27 H26 F12 N2 P2'
_chemical_formula_weight         668.44
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.440(2)
_cell_angle_beta                 88.260(2)
_cell_angle_gamma                85.425(2)
_cell_formula_units_Z            6
_cell_length_a                   13.8836(7)
_cell_length_b                   17.9623(10)
_cell_length_c                   18.7911(10)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.3
_cell_volume                     4520.9(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56115
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
Contribution of disordered molecules of methanol was removed from data.
;
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.710
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         17715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.710
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1961P)^2^+13.1545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2488
_reflns_number_gt                9595
_reflns_number_total             17715
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1sc00468a.txt
_cod_data_source_block           rac-2-pf6
_cod_database_code               1515533