Role of Pyrazine-N,N′-dioxide in [W(CN)8]n−-Based Hybrid Networks: Anion−π Interactions
Podgajny, Robert; Pinkowicz, Dawid; Czarnecki, Bernard; Kozieł, Marcin; Chorąży, Szymon; Wis, Magdalena; Nitek, Wojciech; Rams, Michał; Sieklucka, Barbara; Crystal Growth & Design 14 (2014) 4030–; doi:10.1021/cg500636m

data_4511647
_publ_section_title
;
 Role of Pyrazine-N,N&#x2032;-dioxide in [W(CN)8]n&#x2212;-Based Hybrid
 Networks: Anion&#x2212;\p Interactions
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4030
_journal_paper_doi               10.1021/cg500636m
_journal_volume                  14
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '3K, 2(C4 H4 N2 O2), W C8 N8, 4(H2 O)'
_chemical_formula_sum            'C16 H16 K3 N12 O8 W'
_chemical_formula_weight         805.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-08-13T16:26:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.57900(10)
_cell_length_b                   25.2880(3)
_cell_length_c                   9.7880(4)
_cell_measurement_reflns_used    7088
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     5341.2(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.896592E-1
_diffrn_orient_matrix_UB_12      0.481901E-1
_diffrn_orient_matrix_UB_13      -0.87403E-2
_diffrn_orient_matrix_UB_21      -0.204766E-1
_diffrn_orient_matrix_UB_22      0.40092E-1
_diffrn_orient_matrix_UB_23      0.109973E-1
_diffrn_orient_matrix_UB_31      0.73534E-2
_diffrn_orient_matrix_UB_32      -0.67408E-2
_diffrn_orient_matrix_UB_33      0.382663E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3906
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.859
_exptl_absorpt_correction_T_max  0.7932
_exptl_absorpt_correction_T_min  0.7273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3127
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.85
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.386(5)
_refine_ls_extinction_coef       0.000325(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.1
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0069P)^2^+25.0708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                3766
_reflns_number_total             3906
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg500636m_si_002.cif
_cod_data_source_block           mk103
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4511646--4511649.cif.
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_cod_database_code               4511647