Calix[6]azacryptand Ligand with a Sterically Protected Tren-Based Coordination Site for Metal Ions.
Zahim, Sara; Wickramasinghe, Lasantha A.; Evano, Gwilherm; Jabin, Ivan; Schrock, Richard R.; Müller, Peter; Organic letters 18 (2016) 1570–1573; doi:10.1021/acs.orglett.6b00410

data_1543015
_publ_section_title
;
 Calix[6]azacryptand Ligand with a Sterically Protected Tren-Based
 Coordination Site for Metal Ions.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1570
_journal_page_last               1573
_journal_paper_doi               10.1021/acs.orglett.6b00410
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C67 H86 Cl2 N4 O6'
_chemical_formula_weight         1114.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                96.938(2)
_cell_angle_beta                 95.935(2)
_cell_angle_gamma                92.1575(19)
_cell_formula_units_Z            2
_cell_length_a                   10.6524(10)
_cell_length_b                   11.9315(13)
_cell_length_c                   23.654(3)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.37
_cell_measurement_theta_min      2.29
_cell_volume                     2964.6(6)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            99187
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         1.722
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         16616
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+1.7349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12091
_reflns_number_total             16616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b00410_si_002.cif
_cod_data_source_block           x15122
_cod_original_cell_volume        2964.5(5)
_cod_database_code               1543015
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2014/6
_shelx_res_checksum              33353
_shelx_hkl_checksum              91933