Shaping of calix[4]arenes via double bridging of the upper rim
Slavík, Petr; Eigner, Václav; Lhoták, Pavel; CrystEngComm 18 (2016) 4964–; doi:10.1039/C6CE00314A

data_7224458
_publ_section_title
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 Shaping of calix[4]arenes via double bridging of the upper rim
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_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4964
_journal_paper_doi               10.1039/C6CE00314A
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H44 O6, 0.536(C H2 Cl2)'
_chemical_formula_sum            'C42.54 H45.07 Cl1.07 O6'
_chemical_formula_weight         690.30
_space_group_IT_number           113
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-02-03 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8543(10)
_cell_length_b                   13.8543(10)
_cell_length_c                   9.9079(10)
_cell_measurement_reflns_used    6000
_cell_measurement_temperature    180
_cell_measurement_theta_max      76
_cell_measurement_theta_min      5
_cell_volume                     1901.7(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10619
_diffrn_reflns_theta_full        69.837
_diffrn_reflns_theta_max         75.910
_diffrn_reflns_theta_min         4.463
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             732.997
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.290
_refine_diff_density_max         0.20
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details 'Flack (1983), 871 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2047
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.0078419
_refine_ls_shift/su_mean         0.0001567
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.222E+04 0.373E+04 0.225E+04 908. 196. 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1459
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1459
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                1848
_reflns_number_total             2057
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0622
_oxford_refine_ls_scale          6.0(2)
_oxford_reflns_number_all        2047
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c6ce00314a2.cif
_cod_data_source_block           8_PE456_2_4
_cod_depositor_comments
'Adding full bibliography for 7224456--7224459.cif.'
_cod_original_sg_symbol_Hall     'P -4 2ab '
_cod_original_sg_symbol_H-M      'P -4 21 m '
_cod_database_code               7224458
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
EQUIVALENCE PART(2001, OCC) 
WEIGHT -1 PART(1002, OCC) 
CONT ENANTIO 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1122,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) H   (1132,X'S) 
RIDE C   ( 114,X'S) H   (1143,X'S) H   (1142,X'S) H   (1141,X'S) 
RIDE C   ( 901,X'S) H   (9011,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
DISTANCE 1.460000 , 0.005000 = O(11) TO C(12) 
DISTANCE 1.510000 , 0.005000 = C(12) TO C(13) 
DISTANCE 1.540000 , 0.005000 = C(13) TO C(14) 
ANGLE 109.000000 , 1.000000 = O(11) TO C(12) TO C(13) 
ANGLE 109.000000 , 1.000000 = C(12) TO C(13) TO C(14) 
DISTANCE 1.460000 , 0.005000 = O(11) TO C(112) 
DISTANCE 1.510000 , 0.005000 = C(112) TO C(113) 
DISTANCE 1.540000 , 0.005000 = C(113) TO C(114) 
ANGLE 109.000000 , 1.000000 = O(11) TO C(112) TO C(113) 
ANGLE 109.000000 , 1.000000 = C(112) TO C(113) TO C(114) 
U(IJ)'S  0.0, 0.010000 = O(11) TO C(12) 
U(IJ)'S  0.0, 0.010000 = O(11) TO C(13) 
U(IJ)'S  0.0, 0.010000 = O(11) TO C(14) 
U(IJ)'S  0.0, 0.010000 = O(11) TO C(112) 
U(IJ)'S  0.0, 0.010000 = O(11) TO C(113) 
U(IJ)'S  0.0, 0.010000 = O(11) TO C(114) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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