Metallosupramolecular Architectures of Pseudoterpyridine-Type Ligands and ZnIIMetal Ions
Dumitru, Florina; Legrand, Yves-Marie; Barboiu, Mihail; Petit, Eddy; Lee, Arie van der; Crystal Growth & Design 9 (2009) 2917–; doi:10.1021/cg9002466

data_4509524
_publ_section_title
;
 Metallosupramolecular Architectures of Pseudoterpyridine-Type Ligands and
 ZnIIMetal Ions
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2917
_journal_paper_doi               10.1021/cg9002466
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C38 H34 N10 Zn, 2(C F3 O3 S)'
_chemical_formula_sum            'C40 H34 F6 N10 O6 S2 Zn'
_chemical_formula_weight         994.30
_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
_cell_angle_alpha                90
_cell_angle_beta                 96.844(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3943(3)
_cell_length_b                   16.2129(4)
_cell_length_c                   19.7183(5)
_cell_measurement_reflns_used    9587
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.4217
_cell_measurement_theta_min      2.7084
_cell_volume                     4251.52(18)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.4205
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details
;
  1 omega  -54.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000    0.0000    0.0000    0.0000 115

  2 omega  -54.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000   90.0000    0.0000    0.0000 115

  3 omega  -54.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000  180.0000    0.0000    0.0000 115

  4 omega  -54.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000  270.0000    0.0000    0.0000 115

  5 omega -111.00   10.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -25.0000  -80.0000  100.0000    0.0000    0.0000 121

  6 omega -116.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -25.0000  -10.0000  180.0000    0.0000    0.0000 187

  7 omega -110.00   12.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -25.0000  -80.0000    0.0000    0.0000    0.0000 122

;
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.0377618766
_diffrn_orient_matrix_UB_12      0.0250073625
_diffrn_orient_matrix_UB_13      0.0179707870
_diffrn_orient_matrix_UB_21      0.0260201799
_diffrn_orient_matrix_UB_22      -0.0359059037
_diffrn_orient_matrix_UB_23      0.0128745298
_diffrn_orient_matrix_UB_31      0.0272765567
_diffrn_orient_matrix_UB_32      -0.0004154205
_diffrn_orient_matrix_UB_33      -0.0287383130
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_sigmaI/netI    0.1252
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41655
_diffrn_reflns_theta_full        30.243
_diffrn_reflns_theta_max         32.519
_diffrn_reflns_theta_min         2.720
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.17
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3688
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.000274
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 5.46 -5.73 2.92 -0.541 -0.814 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0736
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0526
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                3688
_reflns_number_total             7018
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0587
_oxford_refine_ls_scale          0.7148(11)
_oxford_reflns_number_all        7018
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            cg9002466sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4509524