#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:34:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179336 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/33/4323376.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_4323376
loop_
_publ_author_name
'Philip J. Blower'
'John C. Jeffery'
'John R. Miller'
'Spencer N. Salek'
'Dirk Schmaljohann'
'Raymond J. Smith'
'Michael J. Went'
_publ_contact_author
;
    Dr. J.R. Miller
    Dept. of Biological and Chemical Sciences
    Central Campus
    University of Essex
    Wivenhoe Park
    Colchester  CO4 3SQ
    UK
;
_publ_contact_author_email       john@essex.ac.uk
_publ_contact_author_phone       '01206 87 2117'
_publ_section_title
;
 Template Synthesis and Reactions of Tricarbonylmolybdenum
 Phosphadithiamacrocycle Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1578
_journal_page_last               1582
_journal_paper_doi               10.1021/ic961143i
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C20 H26 Mo P2 S4'
_chemical_formula_weight         552.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                100.29(2)
_cell_angle_beta                 99.775(15)
_cell_angle_gamma                98.81(2)
_cell_formula_units_Z            2
_cell_length_a                   8.105(3)
_cell_length_b                   8.263(3)
_cell_length_c                   17.663(4)
_cell_measurement_temperature    173(2)
_cell_volume                     1126.3(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5355
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    1.100
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0270(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.151
_refine_ls_goodness_of_fit_obs   1.148
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_restrained_S_obs      1.148
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_obs          0.0201
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0205P)²+1.0660P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0516
_refine_ls_wR_factor_obs         0.0505
_reflns_number_observed          3737
_reflns_number_total             3810
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961143i_1.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+1.0660P] 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^)+(0.0205P)^2^+1.0660P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1126.4(6)
_cod_database_code               4323376
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo Mo 0.31868(2) 0.61466(2) 0.223548(9) 0.01494(8) Uani 1 d . .
P1 P 0.25076(6) 0.31958(6) 0.15051(3) 0.01761(12) Uani 1 d . .
P2 P 0.15202(7) 0.65489(7) 0.32773(3) 0.01925(12) Uani 1 d . .
S11 S 0.41964(6) 0.65883(7) 0.11107(3) 0.02184(12) Uani 1 d . .
S12 S 0.48151(6) 0.48735(6) 0.31183(3) 0.02174(12) Uani 1 d . .
S21 S 0.49603(7) 0.86064(6) 0.29964(3) 0.02288(12) Uani 1 d . .
S22 S 0.05587(6) 0.63949(7) 0.15040(3) 0.02241(12) Uani 1 d . .
C111 C 0.3048(3) 0.4833(3) 0.03083(12) 0.0238(4) Uani 1 d . .
H11A H 0.1876(22) 0.4944(3) 0.0172(3) 0.029 Uiso 1 calc R .
H11B H 0.3543(9) 0.4867(3) -0.0148(9) 0.029 Uiso 1 calc R .
C112 C 0.3126(3) 0.3160(3) 0.05448(13) 0.0257(5) Uani 1 d . .
H11C H 0.4241(22) 0.2945(5) 0.05760(14) 0.031 Uiso 1 calc R .
H11D H 0.2384(15) 0.2296(17) 0.0161(8) 0.031 Uiso 1 calc R .
C113 C 0.3774(3) 0.1917(3) 0.20216(14) 0.0263(5) Uani 1 d . .
H11E H 0.3204(12) 0.0824(22) 0.1904(3) 0.032 Uiso 1 calc R .
H11F H 0.4801(21) 0.1942(3) 0.1864(4) 0.032 Uiso 1 calc R .
C114 C 0.4075(3) 0.2614(3) 0.29040(14) 0.0278(5) Uani 1 d . .
H11G H 0.4898(16) 0.2105(11) 0.3171(6) 0.033 Uiso 1 calc R .
H11H H 0.3051(20) 0.2364(6) 0.3083(4) 0.033 Uiso 1 calc R .
C121 C 0.0330(3) 0.2025(2) 0.12781(12) 0.0203(4) Uani 1 d . .
C122 C -0.0272(3) 0.1105(3) 0.17941(14) 0.0274(5) Uani 1 d . .
H122 H 0.0413(24) 0.1030(4) 0.2212(14) 0.033 Uiso 1 calc R .
C123 C -0.1969(3) 0.0305(3) 0.16440(14) 0.0309(5) Uani 1 d . .
H123 H -0.2367(13) -0.0318(19) 0.1997(11) 0.037 Uiso 1 calc R .
C124 C -0.3068(3) 0.0423(3) 0.09773(14) 0.0295(5) Uani 1 d . .
H124 H -0.4177(36) -0.0094(17) 0.0880(3) 0.035 Uiso 1 calc R .
C125 C -0.2489(3) 0.1321(3) 0.04614(15) 0.0319(5) Uani 1 d . .
H125 H -0.3245(24) 0.1397(4) 0.0007(15) 0.038 Uiso 1 calc R .
C126 C -0.0795(3) 0.2118(3) 0.06050(14) 0.0272(5) Uani 1 d . .
H126 H -0.0428(12) 0.2691(19) 0.0265(11) 0.033 Uiso 1 calc R .
C211 C 0.4522(3) 0.8860(3) 0.39964(13) 0.0275(5) Uani 1 d . .
H21A H 0.5083(12) 0.8123(15) 0.4269(6) 0.033 Uiso 1 calc R .
H21B H 0.4990(10) 0.9991(22) 0.4277(6) 0.033 Uiso 1 calc R .
C212 C 0.2619(3) 0.8483(3) 0.39980(13) 0.0272(5) Uani 1 d . .
H21C H 0.2142(10) 0.9357(18) 0.3882(3) 0.033 Uiso 1 calc R .
H21D H 0.2475(4) 0.8369(3) 0.4486(10) 0.033 Uiso 1 calc R .
C213 C -0.0603(3) 0.6932(3) 0.28886(13) 0.0271(5) Uani 1 d . .
H21E H -0.1390(16) 0.6546(8) 0.3186(6) 0.033 Uiso 1 calc R .
H21F H -0.0563(3) 0.8094(23) 0.2924(2) 0.033 Uiso 1 calc R .
C214 C -0.1166(3) 0.6006(3) 0.20332(14) 0.0290(5) Uani 1 d . .
H21G H -0.2126(20) 0.6371(8) 0.1796(5) 0.035 Uiso 1 calc R .
H21H H -0.1466(7) 0.4854(24) 0.20094(15) 0.035 Uiso 1 calc R .
C221 C 0.1119(3) 0.4928(3) 0.38405(13) 0.0234(4) Uani 1 d . .
C222 C -0.0289(3) 0.3629(3) 0.35595(15) 0.0310(5) Uani 1 d . .
H222 H -0.1067(26) 0.3636(3) 0.3105(15) 0.037 Uiso 1 calc R .
C223 C -0.0543(4) 0.2324(3) 0.3951(2) 0.0386(6) Uani 1 d . .
H223 H -0.1431(33) 0.1489(31) 0.3763(7) 0.046 Uiso 1 calc R .
C224 C 0.0578(4) 0.2322(3) 0.4631(2) 0.0397(6) Uani 1 d . .
H224 H 0.0399(7) 0.1442(31) 0.4896(9) 0.048 Uiso 1 calc R .
C225 C 0.1967(4) 0.3616(3) 0.4923(2) 0.0374(6) Uani 1 d . .
H225 H 0.2701(27) 0.3621(3) 0.5377(16) 0.045 Uiso 1 calc R .
C226 C 0.2244(3) 0.4902(3) 0.45255(14) 0.0309(5) Uani 1 d . .
H226 H 0.3175(30) 0.5743(27) 0.4716(6) 0.037 Uiso 1 calc R .
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'
Mo Mo -1.6832 0.6857 '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
S11 Mo S21 91.62(3) . . ?
S11 Mo S22 83.64(3) . . ?
S21 Mo S22 117.48(3) . . ?
S11 Mo S12 117.93(3) . . ?
S21 Mo S12 82.94(3) . . ?
S22 Mo S12 151.07(2) . . ?
S11 Mo P2 157.23(2) . . ?
S21 Mo P2 83.38(3) . . ?
S22 Mo P2 79.10(3) . . ?
S12 Mo P2 83.60(3) . . ?
S11 Mo P1 82.35(3) . . ?
S21 Mo P1 155.58(2) . . ?
S22 Mo P1 85.49(3) . . ?
S12 Mo P1 79.15(3) . . ?
P2 Mo P1 110.73(3) . . ?
C121 P1 C113 105.02(10) . . ?
C121 P1 C112 105.18(10) . . ?
C113 P1 C112 107.43(11) . . ?
C121 P1 Mo 120.48(7) . . ?
C113 P1 Mo 110.53(8) . . ?
C112 P1 Mo 107.50(7) . . ?
C221 P2 C213 104.71(11) . . ?
C221 P2 C212 106.51(11) . . ?
C213 P2 C212 105.75(11) . . ?
C221 P2 Mo 120.29(7) . . ?
C213 P2 Mo 111.17(8) . . ?
C212 P2 Mo 107.47(8) . . ?
C111 S11 Mo 106.45(7) . . ?
C114 S12 Mo 111.17(8) . . ?
C211 S21 Mo 107.72(8) . . ?
C214 S22 Mo 111.33(8) . . ?
C112 C111 S11 111.18(15) . . ?
C111 C112 P1 110.08(15) . . ?
C114 C113 P1 108.8(2) . . ?
C113 C114 S12 110.1(2) . . ?
C122 C121 C126 118.7(2) . . ?
C122 C121 P1 120.8(2) . . ?
C126 C121 P1 120.4(2) . . ?
C121 C122 C123 120.6(2) . . ?
C124 C123 C122 119.8(2) . . ?
C125 C124 C123 120.1(2) . . ?
C124 C125 C126 120.4(2) . . ?
C125 C126 C121 120.3(2) . . ?
C212 C211 S21 112.6(2) . . ?
C211 C212 P2 111.7(2) . . ?
C214 C213 P2 108.7(2) . . ?
C213 C214 S22 110.2(2) . . ?
C226 C221 C222 118.7(2) . . ?
C226 C221 P2 121.5(2) . . ?
C222 C221 P2 119.7(2) . . ?
C223 C222 C221 120.4(2) . . ?
C224 C223 C222 120.2(3) . . ?
C223 C224 C225 120.0(2) . . ?
C224 C225 C226 120.0(3) . . ?
C225 C226 C221 120.7(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
Mo S11 2.3386(7) . ?
Mo S21 2.3404(10) . ?
Mo S22 2.3544(9) . ?
Mo S12 2.3648(8) . ?
Mo P2 2.4666(8) . ?
Mo P1 2.4772(10) . ?
P1 C121 1.820(2) . ?
P1 C113 1.833(2) . ?
P1 C112 1.845(2) . ?
P2 C221 1.828(2) . ?
P2 C213 1.838(2) . ?
P2 C212 1.849(2) . ?
S11 C111 1.840(2) . ?
S12 C114 1.821(2) . ?
S21 C211 1.842(2) . ?
S22 C214 1.828(2) . ?
C111 C112 1.520(3) . ?
C113 C114 1.526(3) . ?
C121 C122 1.390(3) . ?
C121 C126 1.392(3) . ?
C122 C123 1.391(3) . ?
C123 C124 1.379(4) . ?
C124 C125 1.372(4) . ?
C125 C126 1.389(3) . ?
C211 C212 1.527(3) . ?
C213 C214 1.524(3) . ?
C221 C226 1.391(3) . ?
C221 C222 1.394(3) . ?
C222 C223 1.389(4) . ?
C223 C224 1.378(4) . ?
C224 C225 1.383(4) . ?
C225 C226 1.385(4) . ?
