Meta-arylation of calixarenes using organomercurial chemistry.
Slavík, Petr; Flídrová, Karolína; Dvořáková, Hana; Eigner, Václav; Lhoták, Pavel; Organic & biomolecular chemistry 11 (2013) 5528–5534; doi:10.1039/c3ob41085d

data_7153048
_publ_section_title
;
 Meta-arylation of calixarenes using organomercurial chemistry.
;
_journal_issue                   33
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5528
_journal_page_last               5534
_journal_paper_doi               10.1039/c3ob41085d
_journal_volume                  11
_journal_year                    2013
_chemical_formula_moiety         'C80 H94 O8'
_chemical_formula_sum            'C80 H94 O8'
_chemical_formula_weight         1183.62
_space_group_IT_number           14
_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
_cell_angle_alpha                90
_cell_angle_beta                 92.7714(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4473(2)
_cell_length_b                   30.0322(5)
_cell_length_c                   16.7673(3)
_cell_measurement_reflns_used    16925
_cell_measurement_temperature    190
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     6763.59(19)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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      190
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35823
_diffrn_reflns_theta_full        69.056
_diffrn_reflns_theta_max         75.886
_diffrn_reflns_theta_min         4.374
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plane
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9574
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         13670
_refine_ls_number_restraints     223
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.0009346
_refine_ls_shift/su_mean         0.0000636
_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:
511. 773. 366. 79.9
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1007
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1007
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              37
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                11048
_reflns_number_total             13723
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            c3ob41085d.txt
_cod_data_source_block           PE_117_1
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_original_cell_volume        6763.55(19)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7153048