Pillar[5]arene derivatives with three different kinds of repeating units: first examples, crystal structures and selective preparation
Pan, Mingguang; Xue, Min; RSC Adv. 4 (2014) 260–; doi:10.1039/C3RA44581J

data_7239296
_publ_section_title
;
 Pillar[5]arene derivatives with three different kinds of repeating units:
 first examples, crystal structures and selective preparation
;
_journal_issue                   1
_journal_name_full               'RSC Adv.'
_journal_page_first              260
_journal_paper_doi               10.1039/C3RA44581J
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C49 H46 O18, C H2 Cl2, 0.25(C6 H14 O)'
_chemical_formula_sum            'C51.5 H51.5 Cl2 O18.25'
_chemical_formula_weight         1033.33
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.024(7)
_cell_angle_beta                 87.960(7)
_cell_angle_gamma                61.290(9)
_cell_formula_units_Z            2
_cell_length_a                   12.2090(11)
_cell_length_b                   12.3468(11)
_cell_length_c                   19.3418(17)
_cell_measurement_reflns_used    2384
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.5183
_cell_measurement_theta_min      3.2561
_cell_volume                     2542.9(5)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16173
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  0.9498
_exptl_absorpt_correction_T_min  0.9100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1081
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
One quarter disordered isopropyl ether solvent were removed 
from the asymmetric unit.
;
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         9255
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1587P)^2^+0.0588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2604
_refine_ls_wR_factor_ref         0.2991
_reflns_number_gt                5263
_reflns_number_total             9255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra44581j.txt
_cod_data_source_block           130618_pmg_71_2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2542.9(4)
_cod_original_formula_sum        'C51.50 H51.50 Cl2 O18.25'
_cod_database_code               7239296