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_4321629
_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            'C22 H47 Cl4 Cu N8 O25.5'
_chemical_formula_weight         1037.01
_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'
_cell_angle_alpha                90.00000
_cell_angle_beta                 97.7420(10)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            8
_cell_length_a                   20.1350(10)
_cell_length_b                   19.2690(10)
_cell_length_c                   19.7740(10)
_cell_measurement_reflns_used    7862
_cell_measurement_temperature    293
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     7602.0(7)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        xtal
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .042
_diffrn_reflns_av_sigmaI/netI    .115
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            88501
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         1.02
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .96
_exptl_absorpt_correction_T_max  .908
_exptl_absorpt_correction_T_min  .807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       prism
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .20
_refine_diff_density_max         2.308
_refine_diff_density_min         -1.488
_refine_ls_goodness_of_fit_all   4.462
_refine_ls_goodness_of_fit_ref   3.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           atomblock
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1467
_refine_ls_number_reflns         11879
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .096
_refine_ls_R_factor_gt           .055
_refine_ls_shift/su_max          .037
_refine_ls_shift/su_mean         .004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .082
_refine_ls_wR_factor_ref         .057
_reflns_d_resolution_high        .728
_reflns_d_resolution_low         19.872
_reflns_limit_h_max              26
_reflns_limit_h_min              0
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -26
_reflns_number_gt                11879
_reflns_number_total             18826
_reflns_threshold_expression     'F    > 3.00 sig(I   )'
_cod_data_source_file            ic000346a_09.cif
_cod_data_source_block           18a11
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_formula_sum        'C22 H47 Cl4 Cu1 N8 O25.5'
_cod_database_code               4321629