Long tailed cage amines: Synthesis, metal complexation, and structure.
Dittrich, Birger; Harrowfield, Jack M.; Koutsantonis, George A.; Nealon, Gareth L.; Skelton, Brian W.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 3433–3448; doi:10.1039/b921930g

data_7024829
_publ_section_title
;
 Long tailed cage amines: Synthesis, metal complexation, and structure.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3433
_journal_page_last               3448
_journal_paper_doi               10.1039/b921930g
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C42 H94 N8, 2(C H4 O),2(H2 O),4(Cl)'
_chemical_formula_sum            'C44 H106 Cl4 N8 O4'
_chemical_formula_weight         953.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-06-11T12:18:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.001(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3572(3)
_cell_length_b                   14.2614(5)
_cell_length_c                   42.0780(10)
_cell_measurement_reflns_used    4095
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2271
_cell_measurement_theta_min      2.4276
_cell_volume                     5584.4(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0256795545
_diffrn_orient_matrix_UB_12      0.0468105596
_diffrn_orient_matrix_UB_13      0.00003935
_diffrn_orient_matrix_UB_21      -0.0687214925
_diffrn_orient_matrix_UB_22      0.0164840287
_diffrn_orient_matrix_UB_23      0.0029723724
_diffrn_orient_matrix_UB_31      0.020357049
_diffrn_orient_matrix_UB_32      -0.003078333
_diffrn_orient_matrix_UB_33      0.0166781686
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1488
_diffrn_reflns_av_unetI/netI     0.3044
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            47180
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         9783
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1965
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1618
_reflns_number_gt                3271
_reflns_number_total             9783
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b921930g.txt
_cod_data_source_block           gk204
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_database_code               7024829