Regioselective alkylation of a methylene group via meta-bridging of calix[4]arenes
Petr Slavik; Hana Dvorakova; Vaclav Eigner; Pavel Lhotak; Chem.Commun. 50 (2014) 10112–; doi:10.1039/C4cc04356A

data_7115537
_publ_section_title
;
 Regioselective alkylation of a methylene group via meta-bridging of
 calix[4]arenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              10112
_journal_paper_doi               10.1039/C4cc04356A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C47 H52 N0 O4'
_chemical_formula_weight         680.9
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                77.854(5)
_cell_angle_beta                 63.909(6)
_cell_angle_gamma                80.759(5)
_cell_formula_units_Z            2
_cell_length_a                   12.3671(7)
_cell_length_b                   12.6350(8)
_cell_length_c                   13.8467(9)
_cell_measurement_reflns_used    3977
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      3.44
_cell_volume                     1894.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.82
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12936
_diffrn_reflns_theta_full        25.89
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.1936
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.44
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.77
_refine_ls_goodness_of_fit_ref   1.64
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    208
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.0476
_refine_ls_shift/su_mean         0.0026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0016I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                6049
_reflns_number_total             8450
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c4cc04356a2.cif
_cod_data_source_block           Ib
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_database_code               7115537