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_4321630
_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            'C40 H96 Cl2 Cu2 N20 O31'
_chemical_formula_weight         1551.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                73.69(2)
_cell_angle_beta                 80.19(3)
_cell_angle_gamma                78.71(2)
_cell_formula_units_Z            1
_cell_length_a                   13.087(3)
_cell_length_b                   12.561(2)
_cell_length_c                   10.499(3)
_cell_measurement_reflns_used    8
_cell_measurement_temperature    293
_cell_measurement_theta_max      16.8
_cell_measurement_theta_min      13.8
_cell_volume                     1612.1(7)
_computing_cell_refinement       'Enraf Nonius software'
_computing_data_collection       'Enraf Nonius software'
_computing_data_reduction        xtal
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  xtal
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type
;
 CAD4 difractometer               
;
_diffrn_measurement_method       '2\q-\w scans'
_diffrn_radiation_detector       'single counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_sigmaI/netI    .033
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5661
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         8
_exptl_absorpt_coefficient_mu    .85
_exptl_absorpt_correction_T_max  .86
_exptl_absorpt_correction_T_min  .65
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 XTAl absorb                    
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          .55
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .2
_refine_diff_density_max         1.179
_refine_diff_density_min         -.673
_refine_ls_extinction_coef       3213(262)
_refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.614
_refine_ls_goodness_of_fit_ref   1.675
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     617
_refine_ls_number_reflns         4519
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .070
_refine_ls_R_factor_gt           .058
_refine_ls_shift/su_max          .085
_refine_ls_shift/su_mean         .006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .064
_refine_ls_wR_factor_ref         .064
_reflns_d_resolution_high        .842
_reflns_d_resolution_low         12.737
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              12
_reflns_limit_l_min              -12
_reflns_number_observed          4519
_reflns_number_total             5661
_reflns_threshold_expression     'I    > 3.00 sig(I   )'
_cod_data_source_file            ic000346a_10.cif
_cod_data_source_block           pd183
_cod_original_sg_symbol_Hall     -p_1
_cod_database_code               4321630