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_7224457
_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 H48 O8, 0.705(C4 H8 O2)'
_chemical_formula_sum            'C44.82 H53.64 O9.41'
_chemical_formula_weight         742.99
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.0803(10)
_cell_length_b                   9.4848(3)
_cell_length_c                   15.2528(5)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    180
_cell_measurement_theta_max      68
_cell_measurement_theta_min      4
_cell_volume                     4207.0(2)
_computing_cell_refinement       'Apex3 (Bruker AXS, 2015)'
_computing_data_collection       'Apex3 (Bruker AXS, 2015)'
_computing_data_reduction        'Apex3 (Bruker AXS, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex3'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31438
_diffrn_reflns_theta_full        68.242
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.039
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1591.437
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.35
_refine_ls_abs_structure_details 'Flack (1983), 3309 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.19(17)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0377
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         7286
_refine_ls_number_restraints     154
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.0007363
_refine_ls_shift/su_mean         0.0000460
_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: 
 3.59 4.78 1.29 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1246
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1246
_reflns_limit_h_max              34
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -18
_reflns_number_gt                7194
_reflns_number_total             7321
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.80
_oxford_diffrn_Wilson_scale      79.06
_oxford_refine_ls_r_factor_ref   0.0522
_oxford_refine_ls_scale          0.11200(5)
_oxford_reflns_number_all        7294
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c6ce00314a2.cif
_cod_data_source_block           7_P518_1
_cod_depositor_comments
'Adding full bibliography for 7224456--7224459.cif.'
_cod_original_sg_symbol_Hall     'P 2c -2ac '
_cod_original_sg_symbol_H-M      'P c a 21 '
_cod_database_code               7224457
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
EQUIVALENCE PART(1001, OCC) 
EQUIVALENCE PART(1002, OCC) 
EQUIVALENCE PART(1003, OCC) 
EQUIVALENCE PART(2001, OCC) 
EQUIVALENCE PART(2002, OCC) 
EQUIVALENCE PART(2003, OCC) 
EQUIVALENCE PART(3001, OCC) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 201,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 312,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 323,X'S) H   ( 322,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 342,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 363,X'S) H   ( 362,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 392,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 402,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 443,X'S) H   ( 442,X'S) H   ( 441,X'S) 
RIDE O   (  47,X'S) H   ( 471,X'S) 
RIDE O   (  49,X'S) H   ( 491,X'S) 
RIDE C   ( 902,X'S) H   (9021,X'S) H   (9022,X'S) H   (9023,X'S) 
RIDE C   ( 905,X'S) H   (9051,X'S) H   (9052,X'S) 
RIDE C   ( 906,X'S) H   (9061,X'S) H   (9062,X'S) H   (9063,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.460000 , 0.005000 = O(37) TO C(38) 
DISTANCE 1.505000 , 0.005000 = C(38) TO C(39) 
DISTANCE 1.540000 , 0.005000 = C(39) TO C(40) 
ANGLE 109.000000 , 1.000000 = O(37) TO C(38) TO C(39) 
ANGLE 109.000000 , 1.000000 = C(38) TO C(39) TO C(40) 
DISTANCE 1.220000 , 0.050000 = C(45) TO O(46) 
DISTANCE 1.290000 , 0.050000 = C(45) TO O(47) 
DISTANCE 1.220000 , 0.050000 = C(45) TO O(146) 
DISTANCE 1.290000 , 0.050000 = C(45) TO O(147) 
DISTANCE 1.220000 , 0.050000 = C(45) TO O(246) 
DISTANCE 1.290000 , 0.050000 = C(45) TO O(247) 
ANGLE 120.000000 , 1.000000 = O(46) TO C(45) TO O(47) 
ANGLE 120.000000 , 1.000000 = O(146) TO C(45) TO O(147) 
ANGLE 120.000000 , 1.000000 = O(246) TO C(45) TO O(247) 
U(IJ)'S  0.0, 0.010000 = C(45) TO O(46) 
U(IJ)'S  0.0, 0.010000 = C(45) TO O(47) 
U(IJ)'S  0.0, 0.010000 = C(45) TO O(146) 
U(IJ)'S  0.0, 0.010000 = C(45) TO O(147) 
U(IJ)'S  0.0, 0.010000 = C(45) TO O(246) 
U(IJ)'S  0.0, 0.010000 = C(45) TO O(247) 
SUM 0.0001 PART(1001, OCC) PART(1002, OCC) PART(1003, OCC) 
DISTANCE 1.220000 , 0.050000 = C(48) TO O(49) 
DISTANCE 1.290000 , 0.050000 = C(48) TO O(50) 
DISTANCE 1.220000 , 0.050000 = C(48) TO O(149) 
DISTANCE 1.290000 , 0.050000 = C(48) TO O(150) 
DISTANCE 1.220000 , 0.050000 = C(48) TO O(249) 
DISTANCE 1.290000 , 0.050000 = C(48) TO O(250) 
ANGLE 120.000000 , 1.000000 = O(49) TO C(48) TO O(50) 
ANGLE 120.000000 , 1.000000 = O(149) TO C(48) TO O(150) 
ANGLE 120.000000 , 1.000000 = O(249) TO C(48) TO O(250) 
U(IJ)'S  0.0, 0.010000 = C(48) TO O(49) 
U(IJ)'S  0.0, 0.010000 = C(48) TO O(50) 
U(IJ)'S  0.0, 0.010000 = C(48) TO O(149) 
U(IJ)'S  0.0, 0.010000 = C(48) TO O(150) 
U(IJ)'S  0.0, 0.010000 = C(48) TO O(249) 
U(IJ)'S  0.0, 0.010000 = C(48) TO O(250) 
SUM 0.0001 PART(2001, OCC) PART(2002, OCC) PART(2003, OCC) 
DISTANCE 1.510000 , 0.005000 = C(901) TO C(902) 
DISTANCE 1.190000 , 0.005000 = C(901) TO O(903) 
DISTANCE 1.310000 , 0.005000 = C(901) TO O(904) 
DISTANCE 1.420000 , 0.005000 = O(904) TO C(905) 
DISTANCE 1.420000 , 0.005000 = C(905) TO C(906) 
ANGLE 123.000000 , 1.000000 = O(903) TO C(901) TO C(902) 
ANGLE 114.000000 , 1.000000 = O(904) TO C(901) TO C(902) 
ANGLE 119.000000 , 1.000000 = C(901) TO O(904) TO C(905) 
ANGLE 109.000000 , 1.000000 = O(904) TO C(905) TO C(906) 
PLANAR 0.010000  C(901) C(902) O(903) O(904) 
DELU 0.01 PART(3001) 
SIMU 0.01 PART(3001) 
END                                                                             
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