Chiral chromane[4]arenes synthesised by cycloaddition reactions of o-quinomethine resorcin[4]arenes
Stefańska, Karolina; Szafraniec, Anna; Szymański, Marek P.; Wierzbicki, Michał; Szumna, Agnieszka; Iwanek, Waldemar; New Journal of Chemistry 43 (2019) 2687–; doi:10.1039/C8NJ06179C

data_7058120
_publ_section_title
;
 Chiral chromane[4]arenes synthesised by cycloaddition reactions of
 o-quinomethine resorcin[4]arenes
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2687
_journal_paper_doi               10.1039/C8NJ06179C
_journal_volume                  43
_journal_year                    2019
_chemical_formula_sum            'C96.15 H112 O8.46'
_chemical_formula_weight         1403.02
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_update_record
;
2018-12-04 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                63.890(2)
_cell_angle_beta                 80.685(2)
_cell_angle_gamma                89.895(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8920(3)
_cell_length_b                   16.9372(4)
_cell_length_c                   17.8109(4)
_cell_measurement_reflns_used    30262
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.3703
_cell_measurement_theta_min      3.7325
_cell_volume                     3968.55(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60538
_diffrn_reflns_theta_full        71.51
_diffrn_reflns_theta_max         71.51
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1510
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1362
_refine_ls_number_reflns         15266
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0984P)^2^+1.3781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1596
_reflns_number_gt                13619
_reflns_number_total             15266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj06179c2.cif
_cod_data_source_block           p_ms
_cod_depositor_comments          'Adding full bibliography for 7058120.cif.'
_cod_original_cell_volume        3968.55(15)
_cod_database_code               7058120