Rearrangement of meta-Bridged Calix[4]arenes Promoted by Internal Strain.
Slavík, Petr; Krupička, Martin; Eigner, Václav; Vrzal, Lukáš; Dvořáková, Hana; Lhoták, Pavel; The Journal of organic chemistry 84 (2019) 4229–4235; doi:10.1021/acs.joc.9b00107

data_4034260
_publ_section_title
;
 Rearrangement of meta-Bridged Calix[4]arenes Promoted by Internal Strain.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4229
_journal_page_last               4235
_journal_paper_doi               10.1021/acs.joc.9b00107
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C32 H30 O4'
_chemical_formula_sum            'C32 H30 O4'
_chemical_formula_weight         478.59
_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     direct
_cell_angle_alpha                90
_cell_angle_beta                 101.5725(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8863(3)
_cell_length_b                   7.2827(2)
_cell_length_c                   24.0141(5)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    120
_cell_measurement_theta_max      49
_cell_measurement_theta_min      12
_cell_volume                     2379.17(10)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.031
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35488
_diffrn_reflns_theta_full        68.294
_diffrn_reflns_theta_max         68.294
_diffrn_reflns_theta_min         3.248
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.605
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.20
_refine_ls_extinction_coef       96(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9510
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4357
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.0014249
_refine_ls_shift/su_mean         0.0001046
_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: 
 4.72 7.14 3.29 0.809 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0887
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0887
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                4031
_reflns_number_total             4357
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.11
_oxford_diffrn_Wilson_scale      47.62
_oxford_refine_ls_r_factor_ref   0.0354
_oxford_refine_ls_scale          0.16627(9)
_oxford_reflns_number_all        4357
_cod_data_source_file            jo9b00107_si_002.cif
_cod_data_source_block           6b
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4034260
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)