Pseudocryptand Hosts for Paraquats and Diquats.
Jones, Jason W.; Price, Jr, Terry L; Huang, Feihe; Zakharov, Lev; Rheingold, Arnold L.; Slebodnick, Carla; Gibson, Harry W.; The Journal of organic chemistry 83 (2018) 823–834; doi:10.1021/acs.joc.7b02812

data_4033325
_publ_section_title
;
 Pseudocryptand Hosts for Paraquats and Diquats.
;
_journal_issue                   2
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              823
_journal_page_last               834
_journal_paper_doi               10.1021/acs.joc.7b02812
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C30 H44 O12, C12 H12 N2, 2(C2 F3 O2), H2 O'
_chemical_formula_sum            'C46 H58 F6 N2 O17'
_chemical_formula_weight         1024.94
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.322(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2302(13)
_cell_length_b                   9.7297(11)
_cell_length_c                   21.768(2)
_cell_measurement_reflns_used    3717
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.54
_cell_measurement_theta_min      2.19
_cell_volume                     2359.1(4)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_type            'Oxford Diffraction Sapphire 3 CCD'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10773
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         4.22
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         4176
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0387P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                3407
_reflns_number_total             4176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7b02812_si_004.cif
_cod_data_source_block           cs725
_cod_depositor_comments
'Adding full bibliography for 4033323--4033325.cif.'
_cod_original_cell_volume        2359.1(5)
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4033325