#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:40:57 +0200 (Thu, 07 Nov 2019) $
#$Revision: 224077 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/82/7048270.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7048270
loop_
_publ_author_name
'Mangelsen, Sebastian'
'Srinivasan, Bikshandarkoil R.'
'Schürmann, Ulrich'
'Kienle, Lorenz'
'Näther, Christian'
'Bensch, Wolfgang'
_publ_section_title
;
 Nanostructured tungsten sulfides: insights into precursor decomposition
 and the microstructure using X-ray scattering methods.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1184
_journal_page_last               1201
_journal_paper_doi               10.1039/c8dt04205e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'H10 N4 S4 W'
_chemical_formula_weight         378.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-10-17 deposited with the CCDC.
2018-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6033(8)
_cell_length_b                   7.4965(8)
_cell_length_c                   18.663(3)
_cell_measurement_reflns_used    3372
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.18
_cell_volume                     923.8(2)
_computing_cell_refinement       'Stadi-4 program package(STOE, 2014)'
_computing_data_collection       'Stadi-4 program package (STOE, 2014)'
_computing_data_reduction        'Stadi-4 program package(STOE, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE Stadi-4 4-circle diffractometer'
_diffrn_measurement_method       'Phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            3372
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.993
_diffrn_reflns_theta_min         2.183
_exptl_absorpt_coefficient_mu    13.341
_exptl_absorpt_correction_T_max  0.2348
_exptl_absorpt_correction_T_min  0.1401
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Stadi-4 program package (STOE, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.719
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Flack x determined using 899 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(9)
_refine_ls_extinction_coef       0.0020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0219P)²+0.2248P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0442
_reflns_Friedel_coverage         0.612
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                2396
_reflns_number_total             2544
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04205e2.cif
_cod_data_source_block           srini43neu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048270--7048271.cif.
;
_cod_database_code               7048270
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
W1 W 0.07330(3) 0.51138(2) 0.87053(2) 0.01902(7) Uani 1 1 d . .
S1 S -0.2269(2) 0.4793(3) 0.91789(8) 0.0328(3) Uani 1 1 d . .
S2 S 0.0483(2) 0.55159(19) 0.75504(8) 0.0285(3) Uani 1 1 d . .
S3 S 0.2286(3) 0.7428(2) 0.91783(9) 0.0305(3) Uani 1 1 d . .
S4 S 0.2551(2) 0.2722(2) 0.89342(9) 0.0276(3) Uani 1 1 d . .
N1 N 0.8642(8) 1.0316(7) 0.9457(3) 0.0349(12) Uani 1 1 d . .
H1N1 H 0.9335 0.9327 0.9578 0.052 Uiso 1 1 d R U
H2N1 H 0.8515 1.1027 0.9843 0.052 Uiso 1 1 d R U
H3N1 H 0.9319 1.0919 0.9115 0.052 Uiso 1 1 d R U
N2 N 0.6694(8) 0.9806(9) 0.9196(3) 0.0388(13) Uani 1 1 d . .
H1N2 H 0.6154 0.8984 0.9491 0.047 Uiso 1 1 d R U
H2N2 H 0.5884 1.0771 0.9177 0.047 Uiso 1 1 d R U
N3 N 0.5858(9) 0.7736(6) 0.7807(3) 0.0294(10) Uani 1 1 d . .
H1N3 H 0.7070 0.8095 0.7641 0.044 Uiso 1 1 d R U
H2N3 H 0.5628 0.6596 0.7679 0.044 Uiso 1 1 d R U
H3N3 H 0.5836 0.7795 0.8289 0.044 Uiso 1 1 d R U
N4 N 0.4297(9) 0.8839(7) 0.7525(3) 0.0366(12) Uani 1 1 d . .
H1N4 H 0.3175 0.8725 0.7795 0.044 Uiso 1 1 d R U
H2N4 H 0.4027 0.8520 0.7070 0.044 Uiso 1 1 d R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
S2 W1 S1 110.26(6)
S2 W1 S4 110.21(6)
S1 W1 S4 109.09(7)
S2 W1 S3 108.82(6)
S1 W1 S3 110.34(7)
S4 W1 S3 108.10(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 S2 2.1826(14)
W1 S1 2.1839(15)
W1 S4 2.1997(15)
W1 S3 2.2000(16)
N1 N2 1.427(8)
N3 N4 1.423(7)
