meta-Bridged Calix[4]arenes Prepared by Friedel–Crafts Alkylation
Slavik, Petr; Dvorakova, Hana; Eigner, Vaclav; Lhotak, Pavel; New Journal of Chemistry 41 (2017) 14738–14745; doi:10.1039/C7NJ03394J

data_7056723
_publ_section_title
;
 meta-Bridged Calix[4]arenes Prepared by Friedel--Crafts Alkylation
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14738
_journal_page_last               14745
_journal_paper_doi               10.1039/C7NJ03394J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C53 H56 O4, 2.45(O) '
_chemical_formula_sum            'C53 H56 O6.45'
_chemical_formula_weight         796.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-06-14 deposited with the CCDC.
2017-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                96.2914(18)
_cell_angle_beta                 92.4769(18)
_cell_angle_gamma                109.769(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0427(3)
_cell_length_b                   11.1946(3)
_cell_length_c                   21.0233(4)
_cell_measurement_reflns_used    21370
_cell_measurement_temperature    120
_cell_measurement_theta_max      67
_cell_measurement_theta_min      4
_cell_volume                     2202.67(10)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_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      120
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36089
_diffrn_reflns_theta_full        67.09
_diffrn_reflns_theta_max         67.094
_diffrn_reflns_theta_min         4.234
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             851.144
_exptl_crystal_size_max          0.586
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9371
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         7769
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.0080923
_refine_ls_shift/su_mean         0.0002911
_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: 
 0.354E+04 0.600E+04 0.372E+04 0.158E+04 361. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1678
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1678
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                6915
_reflns_number_total             7769
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.14
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.0611
_oxford_refine_ls_scale          5.62(12)
_oxford_reflns_number_all        7769
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7nj03394j2.cif
_cod_data_source_block           12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2202.68(10)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C53 H56 O6.45 '
_cod_database_code               7056723
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE C(1, X'S, U'S) UNTIL C(57) 
CONTINUE O(901, X'S, U'S, OCC) UNTIL O(904) 
EQUIVALENCE PART(1001, OCC) 
EQUIVALENCE PART(1002, OCC) 
EQUIVALENCE PART(2001, OCC) 
EQUIVALENCE PART(2002, OCC) 
EQUIVALENCE PART(3001, OCC) 
EQUIVALENCE PART(3002, OCC) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,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   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  16,X'S) H   ( 161,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   ( 201,X'S) H   ( 202,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   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   ( 131,X'S) H   (1311,X'S) H   (1312,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) H   (1322,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) H   (1332,X'S) H   (1333,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) H   (1352,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) H   (1362,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) H   (1372,X'S) H   (1373,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) H   ( 453,X'S) 
RIDE C   ( 143,X'S) H   (1431,X'S) H   (1432,X'S) 
RIDE C   ( 144,X'S) H   (1441,X'S) H   (1442,X'S) 
RIDE C   ( 145,X'S) H   (1451,X'S) H   (1452,X'S) H   (1453,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
END                                                                             
;
_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(42) TO C(43) 
DISTANCE 1.505000 , 0.005000 = C(43) TO C(44) 
DISTANCE 1.540000 , 0.005000 = C(44) TO C(45) 
ANGLE 109.000000 , 1.000000 = O(42) TO C(43) TO C(44) 
ANGLE 109.000000 , 1.000000 = C(43) TO C(44) TO C(45) 
DISTANCE 1.460000 , 0.005000 = O(42) TO C(143) 
DISTANCE 1.505000 , 0.005000 = C(143) TO C(144) 
DISTANCE 1.540000 , 0.005000 = C(144) TO C(145) 
ANGLE 109.000000 , 1.000000 = O(42) TO C(143) TO C(144) 
ANGLE 109.000000 , 1.000000 = C(143) TO C(144) TO C(145) 
U(IJ)'S  0.0, 0.010000 = C(43) TO C(143) 
U(IJ)'S  0.0, 0.010000 = C(44) TO C(144) 
U(IJ)'S  0.0, 0.001000 = C(45) TO C(145) 
SUM 0.0001 PART(1001, OCC) PART(1002, OCC) 
DISTANCE 1.350000 , 0.005000 = C(25) TO O(30) 
DISTANCE 1.460000 , 0.005000 = O(30) TO C(31) 
DISTANCE 1.505000 , 0.005000 = C(31) TO C(32) 
DISTANCE 1.540000 , 0.005000 = C(32) TO C(33) 
ANGLE 109.000000 , 1.000000 = O(30) TO C(31) TO C(32) 
ANGLE 109.000000 , 1.000000 = C(31) TO C(32) TO C(33) 
DISTANCE 1.350000 , 0.005000 = C(25) TO O(130) 
DISTANCE 1.460000 , 0.005000 = O(130) TO C(131) 
DISTANCE 1.505000 , 0.005000 = C(131) TO C(132) 
DISTANCE 1.540000 , 0.005000 = C(132) TO C(133) 
ANGLE 109.000000 , 1.000000 = O(130) TO C(131) TO C(132) 
ANGLE 109.000000 , 1.000000 = C(131) TO C(132) TO C(133) 
U(IJ)'S  0.0, 0.001000 = O(30) TO O(130) 
U(IJ)'S  0.0, 0.010000 = C(31) TO C(131) 
U(IJ)'S  0.0, 0.010000 = C(32) TO C(132) 
U(IJ)'S  0.0, 0.001000 = C(33) TO C(133) 
SUM 0.0001 PART(2001, OCC) PART(2002, OCC) 
DISTANCE 1.460000 , 0.005000 = O(34) TO C(35) 
DISTANCE 1.505000 , 0.005000 = C(35) TO C(36) 
DISTANCE 1.540000 , 0.005000 = C(36) TO C(37) 
ANGLE 109.000000 , 1.000000 = O(34) TO C(35) TO C(36) 
ANGLE 109.000000 , 1.000000 = C(35) TO C(36) TO C(37) 
DISTANCE 1.460000 , 0.005000 = O(34) TO C(135) 
DISTANCE 1.505000 , 0.005000 = C(135) TO C(136) 
DISTANCE 1.540000 , 0.005000 = C(136) TO C(137) 
ANGLE 109.000000 , 1.000000 = O(34) TO C(135) TO C(136) 
ANGLE 109.000000 , 1.000000 = C(135) TO C(136) TO C(137) 
U(IJ)'S  0.0, 0.001000 = C(35) TO C(135) 
U(IJ)'S  0.0, 0.010000 = C(36) TO C(136) 
U(IJ)'S  0.0, 0.010000 = C(37) TO C(137) 
SUM 0.0001 PART(3001, OCC) PART(3002, OCC) 
END                                                                             
;