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_7106691
_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            'C116 H106 Cl6 Cu3 N14 O6'
_chemical_formula_weight         2195.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 106.519(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.308(12)
_cell_length_b                   13.967(7)
_cell_length_c                   32.201(17)
_cell_measurement_reflns_used    562
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.75
_cell_volume                     10050(9)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.2774
_diffrn_reflns_av_sigmaI/netI    0.3645
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            46413
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5535
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4548
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
The unit cell contains an estimated 24 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.

Separate SIMU commands were employed to restraints displacement parameters
on individual aromatic rings. It was also necessary to employ the ISOR command
to restrain the displacment parameters for C14, C22, C36 and C43.
;
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.737
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8817
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      0.736
_refine_ls_R_factor_all          0.2889
_refine_ls_R_factor_gt           0.0779
_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^)+(0.0692P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.2296
_reflns_number_gt                1932
_reflns_number_total             8817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12188j.txt
_cod_data_source_block           cc15
_cod_original_cell_volume        10058(9)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7106691