Closing the cavity: reactive and light switchable dienone-ether macrocycles
Higham, Luke T.; Scott, Janet L.; Strauss, Christopher R.; CrystEngComm 12 (2010) 2803–; doi:10.1039/b926132j

data_7212379
_publ_section_title
;
 Closing the cavity: reactive and light switchable dienone-ether
 macrocycles
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2803
_journal_paper_doi               10.1039/b926132j
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         '(C48 H48 O10)'
_chemical_formula_sum            'C48 H48 O10'
_chemical_formula_weight         784.86
_chemical_name_common
;
(B1),(B2):(B3),(B4)-Bis(ethylene)-(3'E,8E)-3'-(2-(B1)oxy-3-
methoxybenzylidene)-8-(2-(B2)oxy-3-methoxybenzylidene)-3-(2-(B3)oxy-3-
methoxyphenyl)-4-(2-(B4)oxy-3-methoxyphenyl)-3,4,5,6,7,8-
hexahydrospiro(chromene-2,1'-cyclohexan)-2'-one
;
_chemical_name_systematic
;[B1],[B2]:[B3],[B4]-Bis(ethylene)-(3'E,8E)-3'-(2-[B1]oxy-3-methoxybenzylidene)-
8-(2-[B2]oxy-3-methoxybenzylidene)-3-(2-[B3]oxy-3-methoxyphenyl)-4-(2-[B4]oxy-
3-methoxyphenyl)-3,4,5,6,7,8-hexahydrospiro[chromene-2,1'-cyclohexan]-2'-one
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                73.414(1)
_cell_angle_beta                 81.794(1)
_cell_angle_gamma                82.517(1)
_cell_formula_units_Z            2
_cell_length_a                   9.91510(10)
_cell_length_b                   14.0630(2)
_cell_length_c                   14.5961(2)
_cell_measurement_temperature    123(2)
_cell_volume                     1921.96(4)
_computing_cell_refinement       'Nonius collect'
_computing_data_collection       'Nonius collect'
_computing_data_reduction        'Nonius collect'
_computing_molecular_graphics    X-seed
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32621
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_correction_T_min  0.9677
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             832
_exptl_crystal_recrystallization_method 'Slow evaporation from dichloromethane.'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         9291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.7605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                7182
_reflns_number_total             9291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926132j.txt
_cod_data_source_block           intramolecular_Diels_Alder_derivative_of_3
_cod_database_code               7212379