Hybrid[4]arenes with anthracene units and tuneable cavities
Boinski, Tomasz; Szumna, Agnieszka; New J. Chem. 41 (2017) 3387–; doi:10.1039/C7NJ00039A

data_7056088
_publ_section_title
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 Hybrid[4]arenes with anthracene units and tuneable cavities
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              3387
_journal_paper_doi               10.1039/C7NJ00039A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C56 H56 O12, C H Cl3'
_chemical_formula_sum            'C57 H57 Cl3 O12'
_chemical_formula_weight         1040.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-01-02 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 102.451(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6563(10)
_cell_length_b                   17.4377(17)
_cell_length_c                   23.663(3)
_cell_measurement_reflns_used    8910
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.903
_cell_measurement_theta_min      3.826
_cell_volume                     5099.5(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8910
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.903
_diffrn_reflns_theta_min         3.826
_exptl_absorpt_coefficient_mu    2.159
_exptl_crystal_colour            colouless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       prism
_exptl_crystal_F_000             2184
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0004(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.345
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4904
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.355
_refine_ls_R_factor_all          0.1737
_refine_ls_R_factor_gt           0.1234
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3838
_refine_ls_wR_factor_ref         0.4288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2501
_reflns_number_total             4904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00039a2.cif
_cod_data_source_block           tb_ant
_cod_depositor_comments          'Adding full bibliography for 7056088.cif.'
_cod_original_cell_volume        5099.6(10)
_cod_database_code               7056088
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4-C1C = Cl2-C1C = Cl3-C1C
 1.7 with sigma of 0.02
 O22-C34 = O22-C34A
 1.44 with sigma of 0.02
 Cl2-Cl4
 2.7 with sigma of 0.04
 Cl3-Cl4
 2.7 with sigma of 0.04
 Cl3-Cl2
 2.7 with sigma of 0.04
 C24-C34
 2.4 with sigma of 0.04
 C34A-C24
 2.4 with sigma of 0.04
3. Rigid bond restraints
 Cl3, Cl2, C1C, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34, O22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34A, O22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Fixed Sof: Cl3(0.5) Cl2(0.5) C1C(0.5) H1C(0.5) Cl4(0.5)
5.a Ternary CH refined with riding coordinates:
 C1C(H1C)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C21(H21A,H21B)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C15(H15), C20(H20), C23(H23), C29(H29)
5.d Idealised Me refined with riding coordinates:
 C35(H35A,H35B,H35C)
5.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C39(H39A,H39B,H39C), C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              78211
_olex2_submission_special_instructions 'No special instructions were received'