Carboxymethylation of Cage Amines: Control of Alkylation by Metal Ion Coordination
Paul S. Donnelly; Jack M. Harrowfield; Brian W. Skelton; Allan H. White; Inorganic Chemistry 39 (2000) 5817–5830; doi:10.1021/ic000346a

data_4321622
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   Nedlands
   Western Australia 6907
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_9380_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08-9380_3481
_publ_section_title
;
 Carboxymethylation of Cage Amines: Control of Alkylation by Metal Ion
 Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5817
_journal_page_last               5830
_journal_paper_doi               10.1021/ic000346a
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C18 H50 Cl Co N8 O17 S2'
_chemical_formula_weight         809.16
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_cell_angle_beta                 103.40(2)
_cell_angle_gamma                92.050(10)
_cell_formula_units_Z            2
_cell_length_a                   17.937(2)
_cell_length_b                   10.278(3)
_cell_length_c                   10.058(4)
_cell_measurement_reflns_used    8
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.9
_cell_measurement_theta_min      19.0
_cell_volume                     1601.2(9)
_computing_cell_refinement       'Enraf-Nonius software'
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_computing_molecular_graphics    xtal
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_computing_structure_refinement  xtal
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_diffrn_measurement_device_type
;
  CAD4 diffractometer               
;
_diffrn_measurement_method       '2\q-\w scans'
_diffrn_radiation_detector       'single counter'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
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_exptl_absorpt_coefficient_mu    .837
_exptl_absorpt_correction_T_max  .83
_exptl_absorpt_correction_T_min  .79
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 XTAL absorb               
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       prism
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
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_refine_diff_density_max         .674
_refine_diff_density_min         -.975
_refine_ls_extinction_coef       1991(289)
_refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970
_refine_ls_extinction_method     Zachariasen
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_refine_ls_goodness_of_fit_ref   1.771
_refine_ls_hydrogen_treatment    refall
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_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .077
_refine_ls_R_factor_gt           .049
_refine_ls_shift/su_max          .098
_refine_ls_shift/su_mean         .004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .056
_refine_ls_wR_factor_ref         .05
_reflns_d_resolution_high        .77
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_reflns_limit_h_max              23
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_reflns_limit_l_min              -13
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_reflns_number_total             7312
_reflns_threshold_expression     'I    > 3.00 sig(I   )'
_cod_data_source_file            ic000346a_02.cif
_cod_data_source_block           pd50
_cod_original_sg_symbol_Hall     -p_1
_cod_original_formula_sum        'C18 H50 Cl1 Co1 N8 O17 S2'
_cod_database_code               4321622