Calix[4]arenes with intramolecularly bridged meta positions prepared via Pd-catalysed double C-H activation
Jan Holub; Vaclav Eigner; Lukas Vrzal; Hana Dvorakova; Pavel Lhotak; Chem.Commun. 49 (2013) 2798–; doi:10.1039/c3cc40655e

data_7109033
_publ_section_title
;
 Calix[4]arenes with intramolecularly bridged meta positions prepared via
 Pd-catalysed double C-H activation
;
_journal_name_full               Chem.Commun.
_journal_page_first              2798
_journal_paper_doi               10.1039/c3cc40655e
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C45 H51 N1 O4'
_chemical_formula_sum            'C45 H51 N O4'
_chemical_formula_weight         669.9
_chemical_name_systematic        ' ?'
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2ab'
_symmetry_space_group_name_H-M   'P b n 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4797(8)
_cell_length_b                   19.1121(12)
_cell_length_c                   41.8099(15)
_cell_measurement_reflns_used    5866
_cell_measurement_temperature    190
_cell_measurement_theta_max      75.75
_cell_measurement_theta_min      4.66
_cell_volume                     7575.0(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_diffrn_ambient_temperature      190
_diffrn_detector_area_resol_mean 8.1917
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0103
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            32325
_diffrn_reflns_theta_full        76.23
_diffrn_reflns_theta_max         76.23
_diffrn_reflns_theta_min         4.66
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.1744
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.41
_refine_ls_abs_structure_details
' 7049 of Friedel pairs used in the refinement'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    3.28
_refine_ls_goodness_of_fit_ref   2.98
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    841
_refine_ls_number_parameters     944
_refine_ls_number_reflns         24548
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.1117
_refine_ls_shift/su_max          0.0497
_refine_ls_shift/su_mean         0.0016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0025000002F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.1929
_reflns_number_gt                18733
_reflns_number_total             24548
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c3cc40655e.txt
_cod_data_source_block           I
_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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'P -2xab;-2yabc;2zc'
_cod_original_formula_sum        'C45 H51 N1 O4'
_cod_database_code               7109033