#------------------------------------------------------------------------------
#$Date: 2024-11-17 23:40:04 +0200 (Sun, 17 Nov 2024) $
#$Revision: 295979 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/29/4322989.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_4322989
loop_
_publ_author_name
'Scott Chadwick'
'Ulrich Englich'
'Bruce Noll'
'Karin Ruhlandt-Senge'
_publ_section_title
;
 Syntheses and Structure Determinations of Calcium Thiolates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4718
_journal_page_last               4725
_journal_paper_doi               10.1021/ic980086l
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C11 H9 F5 N2 S'
_chemical_formula_weight         296.26
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.261(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1230(4)
_cell_length_b                   28.543(2)
_cell_length_c                   7.2894(5)
_cell_measurement_reflns_used    2608
_cell_measurement_temperature    150(1)
_cell_volume                     1270.44(15)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7814
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        No
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       needle
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.065
_refine_ls_goodness_of_fit_obs   1.183
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_restrained_S_obs      1.183
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_obs          0.0628
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0366P)²+0.3566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1215
_refine_ls_wR_factor_obs         0.0986
_reflns_number_observed          1857
_reflns_number_total             2982
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980086l_5.cif
_cod_data_source_block           Compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2020-11-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1270.45(14)
_cod_original_formula_sum        'C22 H18 F10 N4 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     592.52
_cod_database_code               4322989
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
S1 S -0.33648(11) 0.22171(3) 0.59204(11) 0.0318(2) Uani 1 d . .
F1 F -0.6554(2) 0.14315(6) 0.4989(2) 0.0354(4) Uani 1 d . .
F2 F -0.5976(3) 0.05129(6) 0.5597(2) 0.0404(5) Uani 1 d . .
F3 F -0.2163(3) 0.01864(6) 0.7295(2) 0.0435(5) Uani 1 d . .
F4 F 0.1075(2) 0.08002(6) 0.8398(2) 0.0365(4) Uani 1 d . .
F5 F 0.0521(2) 0.17226(6) 0.7868(2) 0.0333(4) Uani 1 d . .
N1 N 0.1609(4) 0.25964(10) 0.5397(4) 0.0310(6) Uani 1 d . .
N2 N 0.2041(4) 0.35530(9) 0.6480(3) 0.0303(6) Uani 1 d . .
C1 C -0.3039(4) 0.16199(10) 0.6370(3) 0.0241(6) Uani 1 d . .
C2 C -0.4631(4) 0.12874(10) 0.5854(3) 0.0248(6) Uani 1 d . .
C3 C -0.4365(4) 0.08170(10) 0.6149(4) 0.0270(6) Uani 1 d . .
C4 C -0.2444(5) 0.06503(10) 0.7004(4) 0.0286(7) Uani 1 d . .
C5 C -0.0815(4) 0.09624(10) 0.7556(4) 0.0273(6) Uani 1 d . .
C6 C -0.1127(4) 0.14304(10) 0.7259(3) 0.0234(6) Uani 1 d . .
C7 C 0.0429(5) 0.38546(11) 0.6014(4) 0.0315(7) Uani 1 d . .
H7A H -0.0914(5) 0.37343(11) 0.5472(4) 0.038 Uiso 1 calc R .
C8 C 0.0611(5) 0.43303(11) 0.6279(4) 0.0366(8) Uani 1 d . .
H8A H -0.0580(5) 0.45329(11) 0.5931(4) 0.044 Uiso 1 calc R .
C9 C 0.2568(5) 0.45078(12) 0.7063(4) 0.0405(8) Uani 1 d . .
H9A H 0.2751(5) 0.48350(12) 0.7259(4) 0.049 Uiso 1 calc R .
C10 C 0.4243(5) 0.42003(12) 0.7553(4) 0.0379(8) Uani 1 d . .
H10A H 0.5602(5) 0.43113(12) 0.8100(4) 0.045 Uiso 1 calc R .
C11 C 0.3917(5) 0.37331(11) 0.7241(4) 0.0335(7) Uani 1 d . .
H11A H 0.5085(5) 0.35239(11) 0.7581(4) 0.040 Uiso 1 calc R .
H12C H 0.2872(54) 0.2430(12) 0.5643(41) 0.048(10) Uiso 1 d . .
H12B H 0.0244(54) 0.2450(12) 0.5657(42) 0.054(10) Uiso 1 d . .
H12A H 0.1704(52) 0.2920(14) 0.5912(45) 0.058(11) Uiso 1 d . .
H12D H 0.1473(59) 0.2618(14) 0.4040(58) 0.078(13) Uiso 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H12C N1 H12B 117.9(28) . . ?
H12C N1 H12A 112.6(27) . . ?
H12B N1 H12A 110.8(26) . . ?
H12C N1 H12D 103.6(28) . . ?
H12B N1 H12D 102.3(28) . . ?
H12A N1 H12D 108.5(29) . . ?
C7 N2 C11 116.9(3) . . ?
C2 C1 C6 113.9(3) . . ?
C2 C1 S1 123.2(2) . . ?
C6 C1 S1 122.9(2) . . ?
F1 C2 C3 117.3(2) . . ?
F1 C2 C1 119.0(3) . . ?
C3 C2 C1 123.7(2) . . ?
F2 C3 C2 120.5(2) . . ?
F2 C3 C4 119.6(3) . . ?
C2 C3 C4 119.9(3) . . ?
F3 C4 C3 120.4(2) . . ?
F3 C4 C5 120.6(2) . . ?
C3 C4 C5 119.1(3) . . ?
F4 C5 C6 120.8(2) . . ?
F4 C5 C4 119.3(3) . . ?
C6 C5 C4 119.9(2) . . ?
F5 C6 C5 117.2(2) . . ?
F5 C6 C1 119.2(2) . . ?
C5 C6 C1 123.5(2) . . ?
N2 C7 C8 123.4(3) . . ?
N2 C7 H7A 118.3(2) . . ?
C8 C7 H7A 118.3(2) . . ?
C7 C8 C9 118.5(3) . . ?
C7 C8 H8A 120.7(2) . . ?
C9 C8 H8A 120.7(2) . . ?
C10 C9 C8 118.6(3) . . ?
C10 C9 H9A 120.7(2) . . ?
C8 C9 H9A 120.7(2) . . ?
C11 C10 C9 118.9(3) . . ?
C11 C10 H10A 120.6(2) . . ?
C9 C10 H10A 120.6(2) . . ?
N2 C11 C10 123.6(3) . . ?
N2 C11 H11A 118.2(2) . . ?
C10 C11 H11A 118.2(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.744(3) . ?
F1 C2 1.358(3) . ?
F2 C3 1.353(3) . ?
F3 C4 1.350(3) . ?
F4 C5 1.351(3) . ?
F5 C6 1.358(3) . ?
N1 H12C 0.91(3) . ?
N1 H12B 0.97(3) . ?
N1 H12A 1.00(4) . ?
N1 H12D 0.99(4) . ?
N2 C7 1.334(4) . ?
N2 C11 1.340(3) . ?
C1 C2 1.392(4) . ?
C1 C6 1.404(3) . ?
C2 C3 1.368(4) . ?
C3 C4 1.374(4) . ?
C4 C5 1.375(4) . ?
C5 C6 1.364(4) . ?
C7 C8 1.375(4) . ?
C7 H7A 0.95 . ?
C8 C9 1.385(4) . ?
C8 H8A 0.95 . ?
C9 C10 1.377(4) . ?
C9 H9A 0.95 . ?
C10 C11 1.365(4) . ?
C10 H10A 0.95 . ?
C11 H11A 0.95 . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2024-11-17T23:38:10+02:00
;
 Replaced the '&G' character sequence with the backslash character ('\')
 in the '_diffrn_measurement_method' data value.
;
