Hexaphenolic Rigid Cages Prepared by Self-Organization of C<sub>3 v</sub> Tridentates.
Abe, Hajime; Hashikawa, Daisuke; Minami, Takaya; Ohtani, Kohei; Masuda, Kentaro; Matsumoto, Shinya; Inouye, Masahiko; The Journal of organic chemistry 83 (2018) 3132–3141; doi:10.1021/acs.joc.7b03111

data_4033530
_publ_section_title
;
 Hexaphenolic Rigid Cages Prepared by Self-Organization of C<sub>3 v</sub>
 Tridentates.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3132
_journal_page_last               3141
_journal_paper_doi               10.1021/acs.joc.7b03111
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C171 H156 N6 O6 P6 Pd3'
_chemical_formula_sum            'C171 H156 N6 O6 P6 Pd3'
_chemical_formula_weight         2896.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 106.7404(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   27.1507(2)
_cell_length_b                   19.40750(15)
_cell_length_c                   29.4500(2)
_cell_measurement_reflns_used    31608
_cell_measurement_temperature    123
_cell_measurement_theta_max      74.19
_cell_measurement_theta_min      3.01
_cell_volume                     14860.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            83564
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.498
_diffrn_reflns_theta_max         66.498
_diffrn_reflns_theta_min         2.999
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.980
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            clearcolourless
_exptl_crystal_density_diffrn    0.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3000.00
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.097
_refine_diff_density_max         1.92
_refine_diff_density_min         -2.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     877
_refine_ls_number_reflns         26497
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0862P)^2^+25.1158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.1978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22610
_reflns_number_total             26497
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo7b03111_si_002.cif
_cod_data_source_block           xcalibur
_cod_depositor_comments          'Adding full bibliography for 4033530.cif.'
_cod_database_code               4033530
_shelx_res_checksum              9284
_shelx_hkl_checksum              28489
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