2,2′:6′,2″-Terpyridine-4′(1′H)-thione: a missing link in metallosupramolecular chemistry
Constable, Edwin C.; Hermann, B. A.; Housecroft, Catherine E.; Neuburger, Markus; Schaffner, Silvia; Scherer, Lukas J.; New Journal of Chemistry 29 (2005) 1475–; doi:10.1039/b510792j

data_7051566
_publ_section_title
;
 2,2&#x2032;:6&#x2032;,2&#x2033;-Terpyridine-4&#x2032;(1&#x2032;H)-thione:
 a missing link in metallosupramolecular chemistry
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1475
_journal_paper_doi               10.1039/b510792j
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety
;
C120 H80 Fe4 N24 S8, 8(BF4), 5.5(C2H3N), 1.5(C4H10O), CH3O, 4.5(H2O)
;
_chemical_formula_sum            'C138 H123.5 B8 F32 Fe4 N29.5 O7 S8'
_chemical_formula_weight         3481.53
_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
_audit_creation_date             05-07-26
_audit_creation_method           CRYSTALS_ver_12.24
_cell_angle_alpha                90
_cell_angle_beta                 91.118(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.4086(9)
_cell_length_b                   20.1144(8)
_cell_length_c                   34.5052(11)
_cell_measurement_reflns_used    20097
_cell_measurement_temperature    153
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     17631.5(11)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_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    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      153
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.247
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            59868
_diffrn_reflns_theta_full        18.711
_diffrn_reflns_theta_max         24.948
_diffrn_reflns_theta_min         1.760
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             7096
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.30
_refine_diff_density_min         -0.77
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1801
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1272
_refine_ls_number_reflns         10395
_refine_ls_number_restraints     3787
_refine_ls_R_factor_all          0.2783
_refine_ls_R_factor_gt           0.1621
_refine_ls_shift/su_max          0.011809
_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:
2.61 3.12 2.31 0.855 0.527
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2587
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1601
_reflns_limit_h_max              30
_reflns_limit_h_min              -30
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              40
_reflns_limit_l_min              0
_reflns_number_gt                10395
_reflns_number_total             26995
_reflns_threshold_expression     I>1.40u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.0743(2)
_oxford_structure_analysis_title '7130929 ls_a134_153k'
_cod_data_source_file            b510792j.txt
_cod_data_source_block           ls_a134_153k
_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 2.4.1 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      'P 21/n'
_cod_original_formula_sum        'C138 H123.50 B8 F32 Fe4 N29.50 O7 S8'
_cod_database_code               7051566