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_7057693
_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_absolute_configuration ad
_chemical_formula_moiety         'C45 H58 O5'
_chemical_formula_sum            'C45 H58 O5'
_chemical_formula_weight         678.95
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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
;
2018-05-11 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.9267(5)
_cell_length_b                   14.4964(3)
_cell_length_c                   26.1402(7)
_cell_measurement_reflns_used    171
_cell_measurement_temperature    180
_cell_measurement_theta_max      49
_cell_measurement_theta_min      3
_cell_volume                     7929.9(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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.048
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            98268
_diffrn_reflns_theta_full        68.561
_diffrn_reflns_theta_max         68.561
_diffrn_reflns_theta_min         3.048
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2944.005
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_details 'Flack (1983), 6991 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.5(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1132
_refine_ls_number_reflns         14447
_refine_ls_number_restraints     399
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.0109765
_refine_ls_shift/su_mean         0.0005050
_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: 
 4.54 5.98 1.56 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1907
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.1906
_reflns_limit_h_max              25
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              -31
_reflns_number_gt                13893
_reflns_number_total             14459
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.42
_oxford_diffrn_Wilson_scale      150.43
_oxford_refine_ls_r_factor_ref   0.0845
_oxford_refine_ls_scale          0.08919(3)
_oxford_reflns_number_all        14459
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c8nj02577k2.cif
_cod_data_source_block           6a
_cod_depositor_comments
'Adding full bibliography for 7057693--7057697.cif.'
_cod_original_sg_symbol_Hall     'P 2c -2ac '
_cod_original_sg_symbol_H-M      'P c a 21 '
_cod_database_code               7057693