Homonuclear and heteronuclear complexes of a four-armed octadentate ligand: synthetic control based on matching ligand denticity with metal ion coordination preferences
Fenton, Hazel; Tidmarsh, Ian S.; Ward, Michael D.; Dalton Transactions  (2009) 4199–4207; doi:10.1039/b901891c

data_7001307
_publ_section_title
;
 Homonuclear and heteronuclear complexes of a four-armed octadentate
 ligand: synthetic control based on matching ligand denticity with
 metal ion coordination preferences
;
_journal_issue                   21
_journal_name_full               'Dalton Transactions'
_journal_page_first              4199
_journal_page_last               4207
_journal_paper_doi               10.1039/b901891c
_journal_year                    2009
_chemical_formula_sum            'C168 H136 B10 F42 N48 Ni6'
_chemical_formula_weight         4085.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                   29.9778(7)
_cell_length_b                   50.1664(12)
_cell_length_c                   26.2454(6)
_cell_measurement_reflns_used    9591
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.48
_cell_measurement_theta_min      2.22
_cell_volume                     39469.9(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0911
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            342892
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         0.79
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.7780
_exptl_absorpt_correction_T_min  0.6925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             16608
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_platon_squeeze_details
;

The diffraction images showed a lot of diffuse and weak reflectance,
symptomatic of high disorder. This hampered the acquisition of a better data
set in which all the anions could be defined the data. The crystals also
suffered from rapid solvent loss causing almost immediate decomposition when
removed from the mother liquor. Taking these factors into account we feel
that a final R value of 12 % (although higher than would normally be
acceptable) is reasonable for this case.

The pyridyl rings N231 > C236, N371 > C376 and N411 > C416 contain
atoms with higher than average thermal and anisotropic thermal
parameters. This has been reduced by the application of geometric and
displacement restraints. Attempts to split the rings were conducted
but did not yield chemically sensible results (for example the connected
pyrazole rings would have also required splitting, however this was not
required nor successful). In light of this we attribute the problem to
a not totally successful absorption correction most likely due to the
large size of the crystal required for diffraction relative to the beam
diameter.

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.
;
_refine_diff_density_max         2.221
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.440
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2392
_refine_ls_number_reflns         25811
_refine_ls_number_restraints     544
_refine_ls_restrained_S_all      1.455
_refine_ls_R_factor_all          0.1364
_refine_ls_R_factor_gt           0.1151
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3365
_refine_ls_wR_factor_ref         0.3509
_reflns_number_gt                19649
_reflns_number_total             25811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901891c.txt
_cod_data_source_block           imw1223pccn
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'Pccn '
_cod_database_code               7001307