meta-Bridged calix[4]arenes with the methylene moiety possessing in/out stereochemistry of substituents
Slavík, P.; Eigner, V.; Lhoták, P.; New Journal of Chemistry 42 (2018) 16646–; doi:10.1039/C8NJ02577K

data_7057695
_publ_section_title
;
 meta-Bridged calix[4]arenes with the methylene moiety possessing in/out
 stereochemistry of substituents
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16646
_journal_paper_doi               10.1039/C8NJ02577K
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C42 H50 O4'
_chemical_formula_sum            'C42 H50 O4'
_chemical_formula_weight         618.86
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-05-11 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.5755(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.9174(4)
_cell_length_b                   18.1166(4)
_cell_length_c                   18.3273(4)
_cell_measurement_reflns_used    109
_cell_measurement_temperature    180
_cell_measurement_theta_max      45
_cell_measurement_theta_min      5
_cell_volume                     7043.0(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.043
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65644
_diffrn_reflns_theta_full        67.68
_diffrn_reflns_theta_max         68.530
_diffrn_reflns_theta_min         2.083
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2672.003
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         12835
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.0007851
_refine_ls_shift/su_mean         0.0000488
_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: 
 2.06 2.52 0.583 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1196
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1196
_reflns_limit_h_max              25
_reflns_limit_h_min              -26
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                11220
_reflns_number_total             12849
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.63
_oxford_diffrn_Wilson_scale      181.85
_oxford_refine_ls_r_factor_ref   0.0645
_oxford_refine_ls_scale          0.083868(13)
_oxford_reflns_number_all        12848
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c8nj02577k2.cif
_cod_data_source_block           9
_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 

 Adding full bibliography for 7057693--7057697.cif.
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7057695
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) 
EQUIVALENCE PART(1002, OCC) 
EQUIVALENCE PART(2001, OCC) 
EQUIVALENCE PART(2002, 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   ( 142,X'S) H   ( 141,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   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 333,X'S) H   ( 332,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 373,X'S) H   ( 372,X'S) 
RIDE C   ( 235,X'S) H   (2351,X'S) H   (2352,X'S) 
RIDE C   ( 236,X'S) H   (2361,X'S) H   (2362,X'S) 
RIDE C   ( 237,X'S) H   (2372,X'S) H   (2371,X'S) H   (2373,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   ( 412,X'S) H   ( 411,X'S) H   ( 413,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,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   (  46,X'S) H   ( 461,X'S) H   ( 463,X'S) H   ( 462,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) H   (1022,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 108,X'S) H   (1082,X'S) H   (1081,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) H   (1142,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) H   (1202,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) 
RIDE C   ( 129,X'S) H   (1291,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   (1333,X'S) H   (1332,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   (1372,X'S) H   (1371,X'S) H   (1373,X'S) 
RIDE C   ( 139,X'S) H   (1392,X'S) H   (1391,X'S) 
RIDE C   ( 140,X'S) H   (1401,X'S) H   (1402,X'S) 
RIDE C   ( 141,X'S) H   (1412,X'S) H   (1411,X'S) H   (1413,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   ( 343,X'S) H   (3431,X'S) H   (3432,X'S) 
RIDE C   ( 344,X'S) H   (3441,X'S) H   (3442,X'S) 
RIDE C   ( 345,X'S) H   (3451,X'S) H   (3452,X'S) H   (3453,X'S) 
RIDE C   ( 146,X'S) H   (1461,X'S) H   (1462,X'S) H   (1463,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(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(235) 
DISTANCE 1.505000 , 0.005000 = C(235) TO C(236) 
DISTANCE 1.540000 , 0.005000 = C(236) TO C(237) 
ANGLE 109.000000 , 1.000000 = O(34) TO C(235) TO C(236) 
ANGLE 109.000000 , 1.000000 = C(235) TO C(236) TO C(237) 
U(IJ)'S  0.0, 0.010000 = O(34) TO C(35) 
U(IJ)'S  0.0, 0.010000 = O(34) TO C(36) 
U(IJ)'S  0.0, 0.010000 = O(34) TO C(37) 
U(IJ)'S  0.0, 0.010000 = O(34) TO C(235) 
U(IJ)'S  0.0, 0.010000 = O(34) TO C(236) 
U(IJ)'S  0.0, 0.010000 = O(34) TO C(237) 
SUM 0.0001 PART(1001, OCC) PART(1002, OCC) 
DISTANCE 1.460000 , 0.005000 = O(142) 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(142) TO C(143) TO C(144) 
ANGLE 109.000000 , 1.000000 = C(143) TO C(144) TO C(145) 
DISTANCE 1.460000 , 0.005000 = O(142) TO C(343) 
DISTANCE 1.505000 , 0.005000 = C(343) TO C(344) 
DISTANCE 1.540000 , 0.005000 = C(344) TO C(345) 
ANGLE 109.000000 , 1.000000 = O(142) TO C(343) TO C(344) 
ANGLE 109.000000 , 1.000000 = C(343) TO C(344) TO C(345) 
U(IJ)'S  0.0, 0.001000 = C(143) TO C(343) 
U(IJ)'S  0.0, 0.001000 = C(144) TO C(344) 
U(IJ)'S  0.0, 0.001000 = C(145) TO C(345) 
SUM 0.0001 PART(2001, OCC) PART(2002, OCC) 
END                                                                             
;