A tetrapyridine ligand with a rigid tetrahedral core forms metalorganic frameworks with PtS type architecture
Christopher; B.; Caputo,; V.; Nicholas; Vukotic,; Natalie; M.; Sirizzotti; and; Stephen; J.; Loeb; Christopher Caputo; V. Nicholas Vukotic; Natalie Sirizzotti; Stephen Loeb; Chem.Commun. 47 (2011) 8545–; doi:10.1039/c1cc12188j

data_7106692
_publ_section_title
;
 A tetrapyridine ligand with a rigid tetrahedral core forms
 metal&#x0096;organic frameworks with PtS type architecture
;
_journal_name_full               Chem.Commun.
_journal_page_first              8545
_journal_paper_doi               10.1039/c1cc12188j
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C64.5 H77.5 Cl2 Cu N10.5 O6.5'
_chemical_formula_weight         1238.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           50
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2b'
_symmetry_space_group_name_H-M   'P b a n :2'
_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            4
_cell_length_a                   14.995(3)
_cell_length_b                   30.625(7)
_cell_length_c                   14.689(3)
_cell_measurement_reflns_used    364
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.35
_cell_volume                     6746(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'phi and 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  0.1884
_diffrn_reflns_av_sigmaI/netI    0.1299
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60393
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7739
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2612
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
The unit cell contains an estimated 26 molecules of DMF which have
been treated as a diffuse contribution to the overall scattering
without specific atom positions by SQUEEZE/PLATON.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

There was evidence of disorder at the Cu2-Cl2-N13 coordination envoronment.
The largest residual peak is close to Cu2 and there is evidence for
splitting peaks N13 - C18. All attempts to model this disorder with two
sets of CuCl(py) fragments resulted in unstable refinement and/or NPD atoms.
;
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1666
_refine_ls_R_factor_gt           0.0821
_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^)+(0.0914P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                2853
_reflns_number_total             5946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12188j.txt
_cod_data_source_block           cc22o
_cod_original_sg_symbol_H-M      Pban
_cod_database_code               7106692