Synthesis and structure of a zinc(II)-carboxylate trimer containing the π···π stacking, 1,8-naphthalimide synthon: A supramolecular metal–organic framework
Daniel L. Reger; Agota Debreczeni; Mark D. Smith; Inorganica Chimica Acta 364 (2010) 10–15; doi:10.1016/j.ica.2010.05.039

data_1513118
_publ_section_title
;
 Synthesis and structure of a zinc(II)-carboxylate trimer containing the
 \p&#x00B7;&#x00B7;&#x00B7;\p stacking, 1,8-naphthalimide synthon: A
 supramolecular metal--organic framework
;
_journal_issue                   1
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              10
_journal_page_last               15
_journal_paper_doi               10.1016/j.ica.2010.05.039
_journal_volume                  364
_journal_year                    2010
_chemical_formula_moiety         'C94 H76 N6 O28 Zn3'
_chemical_formula_sum            'C94 H76 N6 O28 Zn3'
_chemical_formula_weight         1933.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.8580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3260(6)
_cell_length_b                   23.2384(13)
_cell_length_c                   15.5072(8)
_cell_measurement_reflns_used    5714
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.117
_cell_measurement_theta_min      2.539
_cell_volume                     3994.4(4)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  'SHELXTL Version 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            58651
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular bar'
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         8189
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                6319
_reflns_number_total             8189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ad11.cif
_cod_data_source_block           ad11m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1513118