#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:48:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179307 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/04/4320434.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_4320434
loop_
_publ_author_name
'Maravanji S. Balakrishna'
'Rashmishree Panda'
'Joel T. Mague'
_publ_section_title
;
 New 10-Membered Inorganic Heterocyclic Diphosphanes,
 PhN(PX)2{(-OC6H2(tBu)2)(μ-S)((tBu)2C6H2O-)} (X = Cl, F). Synthesis and
 Transition Metal Complexes (Molybdenum(0), Ruthenium(II), Palladium(II),
 and Platinum(II)) of Heterocyclic Diphosphanes. Crystal and Molecular
 Structures of the Chloro Derivative,
 PhN(PCl)2{(-OC6H2(tBu)2)(μ-S)((tBu)2C6H2O-)}, and of a Molybdenum(0)
 Complex of the Fluoro Derivative,
 [Mo(CO)3{η3-PhN(PF)2{(-OC6H2(tBu)2)(μ-S)((tBu)2C6H2O-)}-\kP,\kP,\kS}]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5620
_journal_page_last               5625
_journal_paper_doi               10.1021/ic010518j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C37 H45 F2 Mo N O5 P2 S'
_chemical_formula_weight         811.68
_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-97
_cell_angle_alpha                102.382(4)
_cell_angle_beta                 98.894(5)
_cell_angle_gamma                114.284(4)
_cell_formula_units_Z            2
_cell_length_a                   11.7037(7)
_cell_length_b                   12.2971(5)
_cell_length_c                   16.5033(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.40
_cell_measurement_theta_min      15.98
_cell_volume                     2034.5(2)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1987)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1997)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'θ/2θ scans'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8371
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        8.2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_correction_T_min  0.8327
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ψ scan (North, et al., 1968)'
_exptl_crystal_colour            Amber
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0697P)²+0.3386P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                5094
_reflns_number_total             7963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010518j_2.cif
_cod_data_source_block           msb07
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2034.51(18)
_cod_database_code               4320434
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo 0.80608(3) 0.51334(3) 0.72301(2) 0.04140(12) Uani 1 1 d . . .
P1 P 0.64623(9) 0.48444(9) 0.80051(6) 0.0382(2) Uani 1 1 d . . .
P2 P 0.59569(9) 0.45588(9) 0.63840(6) 0.0397(2) Uani 1 1 d . . .
S S 0.70906(9) 0.27936(9) 0.69586(6) 0.0400(2) Uani 1 1 d . . .
F1 F 0.6309(2) 0.5821(2) 0.87231(14) 0.0559(6) Uani 1 1 d . . .
F2 F 0.5450(2) 0.5284(2) 0.58741(14) 0.0569(6) Uani 1 1 d . . .
O1 O 0.5891(2) 0.3662(2) 0.83677(16) 0.0442(6) Uani 1 1 d . . .
O2 O 0.5147(2) 0.3212(2) 0.56441(15) 0.0434(6) Uani 1 1 d . . .
O3 O 0.9411(4) 0.5102(5) 0.5734(3) 0.131(2) Uani 1 1 d . . .
O4 O 0.9123(4) 0.8025(3) 0.7628(2) 0.0827(10) Uani 1 1 d . . .
O5 O 1.0426(4) 0.5453(5) 0.8643(3) 0.1151(16) Uani 1 1 d . . .
N N 0.5193(3) 0.4484(3) 0.71695(18) 0.0378(7) Uani 1 1 d . . .
C1 C 0.6588(3) 0.3029(3) 0.8577(2) 0.0398(8) Uani 1 1 d . . .
C2 C 0.7190(4) 0.2616(4) 0.8011(2) 0.0413(8) Uani 1 1 d . . .
C15 C 0.4654(4) 0.2079(3) 0.5830(2) 0.0398(8) Uani 1 1 d . . .
C20 C 0.5366(3) 0.1831(3) 0.6447(2) 0.0400(8) Uani 1 1 d . . .
C29 C 0.3842(3) 0.4115(4) 0.7142(2) 0.0425(9) Uani 1 1 d . . .
C30 C 0.3322(4) 0.4892(5) 0.6994(3) 0.0652(12) Uani 1 1 d . . .
H30 H 0.3839 0.5655 0.6921 0.078 Uiso 1 1 calc R . .
C31 C 0.2028(5) 0.4535(6) 0.6954(4) 0.0910(18) Uani 1 1 d . . .
H31 H 0.1667 0.5054 0.6843 0.109 Uiso 1 1 calc R . .
C32 C 0.1278(5) 0.3431(6) 0.7075(4) 0.0883(18) Uani 1 1 d . . .
H32 H 0.0410 0.3205 0.7058 0.106 Uiso 1 1 calc R . .
C33 C 0.1790(5) 0.2650(5) 0.7221(3) 0.0723(14) Uani 1 1 d . . .
H33 H 0.1268 0.1890 0.7297 0.087 Uiso 1 1 calc R . .
C34 C 0.3082(4) 0.2987(4) 0.7257(3) 0.0526(10) Uani 1 1 d . . .
H34 H 0.3435 0.2460 0.7357 0.063 Uiso 1 1 calc R . .
C35 C 0.8940(4) 0.5105(4) 0.6284(3) 0.0688(14) Uani 1 1 d . . .
C36 C 0.8750(4) 0.6969(4) 0.7491(3) 0.0536(10) Uani 1 1 d . . .
C37 C 0.9587(4) 0.5361(4) 0.8129(3) 0.0641(12) Uani 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'
O O 0.0106 0.0060 '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'
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'
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
C36 Mo C35 89.71(19) . . ?
C36 Mo C37 91.28(19) . . ?
C35 Mo C37 94.0(2) . . ?
C36 Mo P2 97.15(13) . . ?
C35 Mo P2 98.31(15) . . ?
C37 Mo P2 165.07(15) . . ?
C36 Mo P1 96.44(13) . . ?
C35 Mo P1 163.15(14) . . ?
C37 Mo P1 101.49(14) . . ?
P2 Mo P1 65.42(3) . . ?
C36 Mo S 176.40(12) . . ?
C35 Mo S 93.82(14) . . ?
C37 Mo S 89.17(14) . . ?
P2 Mo S 81.66(3) . . ?
P1 Mo S 79.98(3) . . ?
F1 P1 O1 97.62(13) . . ?
F1 P1 N 100.70(14) . . ?
O1 P1 N 102.15(14) . . ?
F1 P1 Mo 130.80(11) . . ?
O1 P1 Mo 122.49(10) . . ?
N P1 Mo 97.50(10) . . ?
F1 P1 P2 126.37(10) . . ?
O1 P1 P2 121.34(11) . . ?
N P1 P2 40.43(10) . . ?
Mo P1 P2 57.07(3) . . ?
F2 P2 O2 95.51(13) . . ?
F2 P2 N 103.15(14) . . ?
O2 P2 N 106.47(14) . . ?
F2 P2 Mo 130.89(10) . . ?
O2 P2 Mo 119.88(11) . . ?
N P2 Mo 98.26(10) . . ?
F2 P2 P1 129.34(10) . . ?
O2 P2 P1 124.11(10) . . ?
N P2 P1 40.76(10) . . ?
Mo P2 P1 57.51(3) . . ?
C2 S C20 100.85(17) . . ?
C2 S Mo 104.34(13) . . ?
C20 S Mo 119.01(13) . . ?
C1 O1 P1 123.2(2) . . ?
C15 O2 P2 122.8(2) . . ?
C29 N P2 131.3(2) . . ?
C29 N P1 129.7(2) . . ?
P2 N P1 98.81(15) . . ?
C2 C1 O1 121.4(3) . . ?
C2 C1 C6 120.6(3) . . ?
O1 C1 C6 118.0(3) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 S 115.8(3) . . ?
C1 C2 S 123.5(3) . . ?
C4 C3 C2 120.2(4) . . ?
C5 C4 C3 117.9(4) . . ?
C5 C4 C7 121.7(4) . . ?
C3 C4 C7 120.3(4) . . ?
C4 C5 C6 124.1(4) . . ?
C5 C6 C1 116.3(4) . . ?
C5 C6 C11 120.6(3) . . ?
C1 C6 C11 123.1(3) . . ?
C8 C7 C10 117.5(9) . . ?
C8 C7 C9 105.5(10) . . ?
C10 C7 C9 97.8(7) . . ?
C8 C7 C4 113.0(5) . . ?
C10 C7 C4 114.2(5) . . ?
C9 C7 C4 106.7(6) . . ?
C14 C11 C13 111.2(4) . . ?
C14 C11 C6 109.8(4) . . ?
C13 C11 C6 110.0(4) . . ?
C14 C11 C12 107.6(4) . . ?
C13 C11 C12 107.1(4) . . ?
C6 C11 C12 111.3(4) . . ?
C20 C15 O2 122.6(3) . . ?
C20 C15 C16 120.9(3) . . ?
O2 C15 C16 116.5(3) . . ?
C17 C16 C15 116.1(4) . . ?
C17 C16 C21 121.4(3) . . ?
C15 C16 C21 122.4(4) . . ?
C16 C17 C18 124.1(4) . . ?
C19 C18 C17 117.5(4) . . ?
C19 C18 C25 121.4(4) . . ?
C17 C18 C25 121.1(4) . . ?
C18 C19 C20 121.0(4) . . ?
C15 C20 C19 120.0(3) . . ?
C15 C20 S 124.1(3) . . ?
C19 C20 S 115.7(3) . . ?
C22 C21 C16 109.6(4) . . ?
C22 C21 C23 110.6(4) . . ?
C16 C21 C23 111.4(4) . . ?
C22 C21 C24 106.3(4) . . ?
C16 C21 C24 111.5(4) . . ?
C23 C21 C24 107.3(4) . . ?
C26 C25 C27 111.5(7) . . ?
C26 C25 C18 109.6(5) . . ?
C27 C25 C18 112.6(4) . . ?
C26 C25 C28 110.3(7) . . ?
C27 C25 C28 103.9(6) . . ?
C18 C25 C28 108.8(5) . . ?
C30 C29 C34 120.4(4) . . ?
C30 C29 N 119.3(4) . . ?
C34 C29 N 120.3(4) . . ?
C29 C30 C31 119.6(5) . . ?
C32 C31 C30 120.3(5) . . ?
C31 C32 C33 120.4(5) . . ?
C32 C33 C34 120.1(5) . . ?
C29 C34 C33 119.3(4) . . ?
O3 C35 Mo 177.7(6) . . ?
O4 C36 Mo 178.4(4) . . ?
O5 C37 Mo 177.7(5) . . ?
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 C36 1.977(5) . ?
Mo C35 2.000(5) . ?
Mo C37 2.016(5) . ?
Mo P2 2.3654(10) . ?
Mo P1 2.3770(10) . ?
Mo S 2.5242(10) . ?
P1 F1 1.584(2) . ?
P1 O1 1.618(3) . ?
P1 N 1.693(3) . ?
P1 P2 2.5628(13) . ?
P2 F2 1.567(2) . ?
P2 O2 1.617(3) . ?
P2 N 1.682(3) . ?
S C2 1.788(4) . ?
S C20 1.807(4) . ?
O1 C1 1.393(4) . ?
O2 C15 1.395(4) . ?
O3 C35 1.133(5) . ?
O4 C36 1.143(5) . ?
O5 C37 1.142(5) . ?
N C29 1.445(4) . ?
C1 C2 1.387(5) . ?
C1 C6 1.402(5) . ?
C2 C3 1.384(5) . ?
C3 C4 1.383(6) . ?
C4 C5 1.379(6) . ?
C4 C7 1.540(6) . ?
C5 C6 1.394(5) . ?
C6 C11 1.550(5) . ?
C7 C8 1.363(9) . ?
C7 C10 1.470(9) . ?
C7 C9 1.516(12) . ?
C11 C14 1.531(6) . ?
C11 C13 1.540(6) . ?
C11 C12 1.555(6) . ?
C15 C20 1.380(5) . ?
C15 C16 1.414(5) . ?
C16 C17 1.386(6) . ?
C16 C21 1.536(6) . ?
C17 C18 1.389(6) . ?
C18 C19 1.378(6) . ?
C18 C25 1.533(6) . ?
C19 C20 1.390(5) . ?
C21 C22 1.533(6) . ?
C21 C23 1.538(6) . ?
C21 C24 1.548(6) . ?
C25 C26 1.467(8) . ?
C25 C27 1.522(8) . ?
C25 C28 1.537(8) . ?
C29 C30 1.369(6) . ?
C29 C34 1.379(6) . ?
C30 C31 1.379(7) . ?
C31 C32 1.358(8) . ?
C32 C33 1.367(8) . ?
C33 C34 1.381(6) . ?
