Self-assembly route from a bis-aminal derivative to a new cyclam based macropentacycle
Raphaël Tripier; Stéphanie Develay; Michel Le Baccon; Françoise Chuburu; François Michaud; Henri Handel; New J. Chem. 28 (2004) 173–176; doi:10.1039/b310074j

data_7050198
_publ_section_title
;
 Self-assembly route from a bis-aminal derivative to a new cyclam based
 macropentacycle
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              173
_journal_page_last               176
_journal_paper_doi               10.1039/b310074j
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C20 H30 Br2 N4 O1.75'
_chemical_formula_weight         514.30
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_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.0000(5)
_cell_angle_beta                 90.0000(5)
_cell_angle_gamma                90.0000(5)
_cell_formula_units_Z            16
_cell_length_a                   24.97590(70)
_cell_length_b                   24.97580(70)
_cell_length_c                   16.25780(29)
_cell_measurement_reflns_used    4486
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      2.546
_cell_volume                     10141.5(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1992)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR 97 (Altomar et al., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0298406
_diffrn_orient_matrix_UB_12      -0.0170383
_diffrn_orient_matrix_UB_13      0.0315707
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_diffrn_orient_matrix_UB_22      -0.0065535
_diffrn_orient_matrix_UB_23      -0.0525078
_diffrn_orient_matrix_UB_31      0.0179086
_diffrn_orient_matrix_UB_32      -0.0356350
_diffrn_orient_matrix_UB_33      -0.0054385
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K-alpha'
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    3.216
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   'no correction'
_exptl_crystal_colour            colourless
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_exptl_crystal_description       'truncated octagonal prism'
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.390
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.129
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_restrained_S_obs      1.129
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_obs          0.0695
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+22.1662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2348
_refine_ls_wR_factor_obs         0.1947
_reflns_number_observed          3054
_reflns_number_total             4326
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b310074j.txt
_cod_data_source_block           r3
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+22.1662P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+22.1662P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10141.503(443)
_cod_database_code               7050198