Synthesis of upper rim-double-bridged calix[4]arenes bearing seven membered rings and related compounds
Tlustý, M.; Eigner, V.; Babor, M.; Kohout, M.; Lhoták, P.; RSC Advances 9 (2019) 22017–; doi:10.1039/C9RA05075B

data_7233167
_publ_section_title
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 Synthesis of upper rim-double-bridged calix[4]arenes bearing seven
 membered rings and related compounds
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_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              22017
_journal_paper_doi               10.1039/C9RA05075B
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C44 H49 F3 N2 O5'
_chemical_formula_sum            'C44 H49 F3 N2 O5'
_chemical_formula_weight         742.87
_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     other
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-05-24 deposited with the CCDC.    2019-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.4889(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9434(6)
_cell_length_b                   17.1880(8)
_cell_length_c                   17.1967(8)
_cell_measurement_reflns_used    143
_cell_measurement_temperature    180
_cell_measurement_theta_max      74
_cell_measurement_theta_min      6
_cell_volume                     3971.7(3)
_computing_cell_refinement       'Apex3 (Bruker AXS, 2015)'
_computing_data_collection       'Apex3 (Bruker AXS, 2015)'
_computing_data_reduction        'Apex3 (Bruker AXS, 2015)'
_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      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex3'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56485
_diffrn_reflns_theta_full        68.397
_diffrn_reflns_theta_max         68.397
_diffrn_reflns_theta_min         3.289
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1575.992
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.224
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.40
_refine_ls_extinction_coef       81(13)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         7210
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.0090774
_refine_ls_shift/su_mean         0.0002699
_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: 
 8.42 13.1 6.38 1.62 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1126
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1125
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7016
_reflns_number_total             7283
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.08
_oxford_diffrn_Wilson_scale      88.30
_oxford_refine_ls_r_factor_ref   0.0466
_oxford_refine_ls_scale          0.11434(4)
_oxford_reflns_number_all        7283
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c9ra05075b2.cif
_cod_data_source_block           14a
_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/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7233167