Layered structures and nanosheets of pyrimidinethiolate coordination polymers
P. J. Beldon; S. Tominaka; P. Singh; T. Saha Dasgupta; E. G. Bithell; A. K. Cheetham; Chem.Commun. 50 (2014) 3955–; doi:10.1039/C4CC00771A

data_7112193
_publ_section_title
;
 Layered structures and nanosheets of pyrimidinethiolate coordination
 polymers
;
_journal_name_full               Chem.Commun.
_journal_page_first              3955
_journal_paper_doi               10.1039/C4CC00771A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C8 H6 Fe N4 S2'
_chemical_formula_sum            'C8 H6 Fe N4 S2'
_chemical_formula_weight         278.14
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.90952(17)
_cell_length_b                   16.0335(4)
_cell_length_c                   15.9946(3)
_cell_measurement_reflns_used    5533
_cell_measurement_temperature    293
_cell_measurement_theta_max      70.0340
_cell_measurement_theta_min      5.5000
_cell_volume                     2028.39(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   34.00   76.00   1.0000    1.5900
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   30.0000 42

  2 omega   40.00   77.00   1.0000    1.5900
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -150.0000 37

  3 omega   83.00  126.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  120.0000 43

  4 omega   73.00   98.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  -30.0000 25

  5 omega   41.00  117.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000   60.0000 76

  6 omega   90.00  120.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000    0.0000 30

  7 omega   94.00  120.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000 -150.0000 26

  8 omega   40.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -180.0000 43

  9 omega   37.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  -30.0000 42

 10 omega   42.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   90.0000 28

 11 omega   38.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -60.0000 27

 12 omega   96.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000 -180.0000 26

 13 omega   36.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   30.0000 35

 14 omega   35.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  120.0000 34

 15 omega   56.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000    0.0000 25

 16 omega  102.00  170.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000  -30.0000 68

 17 omega   43.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000  -30.0000 34

 18 omega   38.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000 -180.0000 40

 19 omega   45.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  -90.0000 26

 20 omega   37.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  120.0000 25

 21 omega  -25.00   44.00   1.0000    1.5900
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -150.0000 69

 22 omega  -22.00   69.00   1.0000    1.5900
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 91

 23 omega -124.00  -33.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000 -120.0000 91

 24 omega -124.00  -33.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000  150.0000 91

 25 omega -113.00  -18.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000  120.0000 95

 26 omega -126.00  -23.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000   90.0000 103

 27 omega -126.00  -23.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000  -30.0000 103

 28 omega   73.00  127.00   1.0000    6.3500
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   60.0000 54

 29 omega   36.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000   60.0000 54

 30 omega   36.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000 -120.0000 54
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0414989000
_diffrn_orient_matrix_UB_12      0.0369203000
_diffrn_orient_matrix_UB_13      0.0865528000
_diffrn_orient_matrix_UB_21      -0.1546909000
_diffrn_orient_matrix_UB_22      0.0580542000
_diffrn_orient_matrix_UB_23      -0.0067234000
_diffrn_orient_matrix_UB_31      -0.1107650000
_diffrn_orient_matrix_UB_32      -0.0670807000
_diffrn_orient_matrix_UB_33      0.0417543000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10617
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.234
_diffrn_reflns_theta_min         5.518
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.522
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.2847
_exptl_crystal_size_mid          0.1988
_exptl_crystal_size_min          0.0855
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+0.4429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1699
_reflns_number_total             1928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00771a2.cif
_cod_data_source_block           fepy2th2_rt_slm
_cod_database_code               7112193
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe S2 C8 N4 H6'
_reflns_odcompleteness_completeness 93.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6(0.043) H11(0.048) H1(0.041) H4(0.05) H5(0.047) H7(0.043)
 Fixed X: H6(0.0306) H11(-0.1438) H1(-0.3287) H4(-0.6335) H5(-0.5123) H7(-
 0.4559)
 Fixed Y: H6(0.3136) H11(0.2176) H1(0.142) H4(0.5559) H5(0.458) H7(0.6265)
 Fixed Z: H6(0.7022) H11(0.7696) H1(0.6889) H4(0.3768) H5(0.2897) H7(0.4692)
;
_shelx_res_checksum              19727