Assembly of a Homochiral, Body-Centered Cubic Network Composed of Vertex-Shared Mg12 Cages: Use of Electrospray Ionization Mass Spectrometry to Monitor Metal Carboxylate Nucleation
Jeffrey A. Rood; William C. Boggess; Bruce C. Noll; Kenneth W. Henderson; Journal of the American Chemical Society 129 (2007) 13675–13682; doi:10.1021/ja074558j

data_4110128
_publ_contact_author_address
;University of Notre Dame - Department of Chemistry and Biochemistry
251 Nieuwland Science Hall   Notre Dame, IN 46556-5670
;
_publ_contact_author_email       khenders@nd.edu
_publ_contact_author_fax         '574.631.6652 '
_publ_contact_author_name        'Kenneth W. Henderson'
_publ_contact_author_phone       574.631.7058
_publ_section_title
;
 Assembly of a Homochiral, Body-Centered Cubic Network Composed of
 Vertex-Shared Mg12 Cages: Use of Electrospray Ionization Mass
 Spectrometry to Monitor Metal Carboxylate Nucleation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13675
_journal_page_last               13682
_journal_paper_doi               10.1021/ja074558j
_journal_volume                  129
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H36 Mg2 O15, N O3, C2 H3 N'
_chemical_formula_sum            'C31 H42 Mg2 N2 O18'
_chemical_formula_weight         803.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.87830(10)
_cell_length_b                   19.87830(10)
_cell_length_c                   19.87830(10)
_cell_measurement_reflns_used    5199
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.3178
_cell_measurement_theta_min      3.1437
_cell_volume                     7854.85(7)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2006; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker X8 - ApexII CCD Diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14472
_diffrn_reflns_theta_full        67.80
_diffrn_reflns_theta_max         67.80
_diffrn_reflns_theta_min         3.14
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; Blessing, R.H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2004) SADABS, University of G\:ottingen, Germany
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.423
_exptl_crystal_size_mid          0.411
_exptl_crystal_size_min          0.386
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1234P)^2^+5.3217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                2262
_reflns_number_total             2319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074558jsi20070710_121004.cif
_cod_data_source_block           jr56asq
_cod_original_cell_volume        7854.84(4)
_cod_original_formula_sum        'C31 H42 Mg2  N2 O18'
_cod_database_code               4110128