#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:51:41 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179026 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/24/4122475.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_4122475
loop_
_publ_author_name
'Chitnis, Saurabh S.'
'Whalen, J. Marc'
'Burford, Neil'
_publ_section_title
;
 Influence of charge and coordination number on bond dissociation
 energies, distances, and vibrational frequencies for the
 phosphorus-phosphorus bond.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12498
_journal_page_last               12506
_journal_paper_doi               10.1021/ja507413s
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C4 H12 P2 S2'
_chemical_formula_sum            'C4 H12 P2 S2'
_chemical_formula_weight         186.20
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.020(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   18.657(4)
_cell_length_b                   10.618(2)
_cell_length_c                   6.9703(15)
_cell_measurement_reflns_used    3463
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.93
_cell_volume                     1375.5(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5615
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         2.192
_diffrn_source                   'fine focus sealed X-ray tube'
_diffrn_source_type              'Bruker Krystalloflex 780'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.9469
_exptl_absorpt_correction_T_min  0.8395
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       fragment
_exptl_crystal_F_000             588
_exptl_crystal_recrystallization_method 'grown from CH2Cl2'
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.221
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1658
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0206
_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)+(0.0343P)²+0.2983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1514
_reflns_number_total             1658
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja507413s_si_002.cif
_cod_data_source_block           vic1422
_cod_depositor_comments          'Adding full bibliography for 4122475.cif.'
_cod_database_code               4122475
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2014-3
_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.
;
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.810
_olex2_refinement_description
;
1. Others
 Fixed U12: S4(0) S5(0) P1(0) P2(0) S6(0) P3(0)
 Fixed U23: S4(0) S5(0) P1(0) P2(0) S6(0) P3(0)
 Fixed Y: S4(0.5) S5(0.5) P1(0.5) P2(0.5) S6(0.5) P3(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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
_atom_site_refinement_flags_occupancy
S4 S 0.73831(2) 0.5000 0.67671(6) 0.02926(11) Uani 1 2 d S T P
S5 S 0.92656(2) 0.5000 0.17872(5) 0.02691(11) Uani 1 2 d S T P
P1 P 0.83500(2) 0.5000 0.58779(5) 0.01990(10) Uani 1 2 d S T P
P2 P 0.83013(2) 0.5000 0.26972(5) 0.01889(10) Uani 1 2 d S T P
C7 C 0.88914(7) 0.63587(12) 0.65614(18) 0.0296(2) Uani 1 1 d . . .
H7A H 0.8635(7) 0.7084(14) 0.615(2) 0.041(4) Uiso 1 1 d . . .
H7B H 0.8970(8) 0.6380(15) 0.792(2) 0.043(4) Uiso 1 1 d . . .
H7C H 0.9326(8) 0.6327(14) 0.598(2) 0.048(4) Uiso 1 1 d . . .
C8 C 0.77548(6) 0.36513(11) 0.20031(18) 0.0275(2) Uani 1 1 d . . .
H8A H 0.8001(8) 0.2903(15) 0.246(2) 0.046(4) Uiso 1 1 d . . .
H8B H 0.7689(8) 0.3618(15) 0.065(2) 0.047(4) Uiso 1 1 d . . .
H8C H 0.7312(9) 0.3727(15) 0.249(2) 0.052(5) Uiso 1 1 d . . .
S6 S 0.58770(2) 0.5000 0.30704(5) 0.02760(11) Uani 1 2 d S T P
P3 P 0.49404(2) 0.5000 0.15627(5) 0.01934(10) Uani 1 2 d S T P
C9 C 0.43823(7) 0.36485(12) 0.18936(18) 0.0297(2) Uani 1 1 d . . .
H9A H 0.4636(8) 0.2918(14) 0.168(2) 0.043(4) Uiso 1 1 d . . .
H9B H 0.3963(8) 0.3668(15) 0.099(2) 0.048(4) Uiso 1 1 d . . .
H9C H 0.4264(7) 0.3662(14) 0.319(2) 0.043(4) Uiso 1 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'
P P 0.1023 0.0942 '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'
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
S4 P1 P2 111.05(2) . .
C7 P1 S4 115.29(4) . .
C7 P1 S4 115.29(4) 6_565 .
C7 P1 P2 103.77(4) 6_565 .
C7 P1 P2 103.77(4) . .
C7 P1 C7 106.44(9) 6_565 .
S5 P2 P1 111.49(2) . .
C8 P2 S5 115.32(4) 6_565 .
C8 P2 S5 115.32(4) . .
C8 P2 P1 104.01(4) 6_565 .
C8 P2 P1 104.01(4) . .
C8 P2 C8 105.46(8) 6_565 .
S6 P3 P3 111.53(3) . 5_665
C9 P3 S6 115.48(4) 6_565 .
C9 P3 S6 115.48(4) . .
C9 P3 P3 103.63(4) 6_565 5_665
C9 P3 P3 103.63(4) . 5_665
C9 P3 C9 105.76(9) 6_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S4 P1 1.9580(6) .
S5 P2 1.9591(6) .
P1 P2 2.2110(7) .
P1 C7 1.8012(12) .
P1 C7 1.8012(12) 6_565
P2 C8 1.7994(12) 6_565
P2 C8 1.7994(12) .
S6 P3 1.9588(6) .
P3 P3 2.2091(8) 5_665
P3 C9 1.7996(12) .
P3 C9 1.7996(12) 6_565
