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_1543016
_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            'C68 H89.2 F6 N4 O14.6 S2 Zn'
_chemical_formula_weight         1439.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 109.5763(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5923(12)
_cell_length_b                   26.1314(17)
_cell_length_c                   19.6130(13)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.57
_cell_measurement_theta_min      2.27
_cell_volume                     8495.1(10)
_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 1.000
_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  0.0879
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            209820
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.253
_diffrn_reflns_theta_min         1.228
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1156
_refine_ls_number_reflns         15393
_refine_ls_number_restraints     3030
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0811P)^2^+9.5973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10533
_reflns_number_total             15393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b00410_si_003.cif
_cod_data_source_block           x15151_sq
_cod_original_formula_sum        'C68 H89.20 F6 N4 O14.60 S2 Zn'
_cod_database_code               1543016
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2014/6
_shelx_res_checksum              2960
_shelx_hkl_checksum              51605
_shelx_fab_checksum              81049