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_7233166
_publ_section_title
;
 Synthesis of upper rim-double-bridged calix[4]arenes bearing seven
 membered rings and related compounds
;
_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_absolute_configuration ad
_chemical_formula_moiety         'C54 H53.77 Cl0.24 N2 O4'
_chemical_formula_sum            'C54 H53.77 Cl0.24 N2 O4'
_chemical_formula_weight         803.15
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.5403(3)
_cell_length_b                   14.5403(3)
_cell_length_c                   36.4429(8)
_cell_measurement_reflns_used    160
_cell_measurement_temperature    180
_cell_measurement_theta_max      47
_cell_measurement_theta_min      11
_cell_volume                     6672.5(2)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Venture D8'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            92146
_diffrn_reflns_theta_full        72.100
_diffrn_reflns_theta_max         72.100
_diffrn_reflns_theta_min         3.510
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             2566.635
_exptl_crystal_size_max          0.857
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.236
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details 'Flack (1983), 4298 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         8731
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.0039781
_refine_ls_shift/su_mean         0.0001789
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 4.13P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1007
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1007
_reflns_limit_h_max              0
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              44
_reflns_limit_l_min              -44
_reflns_number_gt                8653
_reflns_number_total             8741
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.29
_oxford_diffrn_Wilson_scale      91.44
_oxford_refine_ls_r_factor_ref   0.0441
_oxford_refine_ls_scale          0.10854(3)
_oxford_reflns_number_all        8731
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c9ra05075b2.cif
_cod_data_source_block           MT_147
_cod_original_cell_volume        6672.5(3)
_cod_original_sg_symbol_H-M      'P 61 '
_cod_database_code               7233166