meta-Bridged calix[4]arenes: a straightforward synthesis via organomercurial chemistry
Karolina Flidrova; Petr Slavik; Vaclav Eigner; Hana Dvorakova; Pavel Lhotak; Chem.Commun. 49 (2013) 6749–; doi:10.1039/c3cc43284j

data_7109541
_publ_section_title
;
 meta-Bridged calix[4]arenes: a straightforward synthesis via
 organomercurial chemistry
;
_journal_name_full               Chem.Commun.
_journal_page_first              6749
_journal_paper_doi               10.1039/c3cc43284j
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C36 H38 O4'
_chemical_formula_sum            'C36 H38 O4'
_chemical_formula_weight         534.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 91.8464(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.09428(16)
_cell_length_b                   15.33790(18)
_cell_length_c                   17.4781(2)
_cell_measurement_reflns_used    31970
_cell_measurement_temperature    293
_cell_measurement_theta_max      76
_cell_measurement_theta_min      5
_cell_volume                     2972.58(6)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_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  0.033
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61451
_diffrn_reflns_theta_full        71.957
_diffrn_reflns_theta_max         75.745
_diffrn_reflns_theta_min         4.654
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0514
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6069
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.0002741
_refine_ls_shift/su_mean         0.0000240
_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:
884. 0.139E+04 674. 157.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1236
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1236
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                5140
_reflns_number_total             6069
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.42
_oxford_diffrn_Wilson_scale      0.07
_oxford_refine_ls_r_factor_ref   0.0709
_oxford_refine_ls_scale          4.58(5)
_oxford_reflns_number_all        6069
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c3cc43284j.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2972.58(7)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7109541
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S)
RIDE C ( 31,X'S) H ( 313,X'S) H ( 311,X'S) H ( 312,X'S)
RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S)
RIDE C ( 34,X'S) H ( 341,X'S) H ( 342,X'S) H ( 343,X'S)
RIDE C ( 36,X'S) H ( 361,X'S) H ( 362,X'S)
RIDE C ( 37,X'S) H ( 371,X'S) H ( 372,X'S) H ( 373,X'S)
RIDE C ( 39,X'S) H ( 392,X'S) H ( 391,X'S)
RIDE C ( 40,X'S) H ( 402,X'S) H ( 401,X'S) H ( 403,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;