#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:19:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179476 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/73/4337370.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_4337370
loop_
_publ_author_name
'Naik, Susmita'
'Kumaravel, Maruthai'
'Mague, Joel T.'
'Balakrishna, Maravanji S.'
_publ_section_title
;
 Novel Trisphosphine Ligand Containing 1,3,5-Triazine Core,
 [2,4,6-C3N3{C6H4PPh2-p}3]: Synthesis and Transition Metal Chemistry.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1370
_journal_page_last               1381
_journal_paper_doi               10.1021/ic402150k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C57 H42 N3 P3 S3, 3(C7 H8)'
_chemical_formula_sum            'C78 H66 N3 P3 S3'
_chemical_formula_weight         1234.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.274(5)
_cell_length_b                   19.274(5)
_cell_length_c                   31.844(8)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.52
_cell_volume                     10245(5)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2009)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω 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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            29541
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_correction_T_min  0.8281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
 A region of density well separated from the remainder of the
 structure and highly disordered about the 3-fold axis was
 removed with the SQUEEZE option of t he PLATON package
 (Spek, 2010).
;
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5169
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0768P)²+9.0816P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1420
_reflns_number_gt                4135
_reflns_number_total             5169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402150k_si_001.cif
_cod_data_source_block           msb495_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4337370
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
S1 S -0.18917(3) 0.78504(3) 0.21528(2) 0.03344(17) Uani 1 1 d . . .
P1 P -0.22418(3) 0.86390(3) 0.218865(16) 0.02061(14) Uani 1 1 d . . .
N1 N -0.62210(9) 0.74874(8) 0.21772(5) 0.0173(3) Uani 1 1 d . . .
C1 C -0.19002(11) 0.93378(12) 0.17508(6) 0.0243(4) Uani 1 1 d . . .
C2 C -0.21022(13) 0.99358(14) 0.17171(7) 0.0325(5) Uani 1 1 d . . .
H2 H -0.2406 1.0001 0.1933 0.039 Uiso 1 1 calc R . .
C3 C -0.18610(14) 1.04358(15) 0.13704(7) 0.0382(5) Uani 1 1 d . . .
H3 H -0.1999 1.0844 0.1349 0.046 Uiso 1 1 calc R . .
C4 C -0.14181(14) 1.03427(15) 0.10543(7) 0.0412(6) Uani 1 1 d . . .
H4 H -0.1264 1.0678 0.0813 0.049 Uiso 1 1 calc R . .
C5 C -0.12035(15) 0.97650(16) 0.10910(8) 0.0430(6) Uani 1 1 d . . .
H5 H -0.0893 0.9708 0.0876 0.052 Uiso 1 1 calc R . .
C6 C -0.14361(13) 0.92625(14) 0.14398(7) 0.0335(5) Uani 1 1 d . . .
H6 H -0.1278 0.8870 0.1465 0.040 Uiso 1 1 calc R . .
C7 C -0.19095(11) 0.92325(11) 0.26645(6) 0.0203(4) Uani 1 1 d . . .
C8 C -0.23079(12) 0.89072(12) 0.30414(6) 0.0263(4) Uani 1 1 d . . .
H8 H -0.2788 0.8403 0.3042 0.032 Uiso 1 1 calc R . .
C9 C -0.20084(12) 0.93146(13) 0.34149(6) 0.0310(5) Uani 1 1 d . . .
H9 H -0.2286 0.9092 0.3670 0.037 Uiso 1 1 calc R . .
C10 C -0.13016(12) 1.00497(13) 0.34176(6) 0.0287(4) Uani 1 1 d . . .
H10 H -0.1093 1.0325 0.3675 0.034 Uiso 1 1 calc R . .
C11 C -0.09026(12) 1.03804(12) 0.30445(6) 0.0276(4) Uani 1 1 d . . .
H11 H -0.0422 1.0884 0.3046 0.033 Uiso 1 1 calc R . .
C12 C -0.12059(11) 0.99747(12) 0.26661(6) 0.0244(4) Uani 1 1 d . . .
H12 H -0.0934 1.0204 0.2410 0.029 Uiso 1 1 calc R . .
C13 C -0.33311(10) 0.81748(11) 0.21880(6) 0.0193(4) Uani 1 1 d . . .
C14 C -0.37114(11) 0.86062(11) 0.22901(6) 0.0216(4) Uani 1 1 d . . .
H14 H -0.3402 0.9153 0.2370 0.026 Uiso 1 1 calc R . .
C15 C -0.45386(11) 0.82406(11) 0.22763(6) 0.0202(4) Uani 1 1 d . . .
H15 H -0.4793 0.8542 0.2338 0.024 Uiso 1 1 calc R . .
C16 C -0.50023(10) 0.74265(10) 0.21712(5) 0.0170(4) Uani 1 1 d . . .
C17 C -0.46202(11) 0.69972(10) 0.20741(6) 0.0194(4) Uani 1 1 d . . .
H17 H -0.4930 0.6446 0.2003 0.023 Uiso 1 1 calc R . .
C18 C -0.37917(11) 0.73644(11) 0.20793(6) 0.0209(4) Uani 1 1 d . . .
H18 H -0.3537 0.7067 0.2009 0.025 Uiso 1 1 calc R . .
C19 C -0.58857(10) 0.70255(10) 0.21758(5) 0.0164(4) Uani 1 1 d . . .
C20 C 0.43899(11) 0.42188(9) 0.26919(7) 0.0390(8) Uani 0.888(3) 1 d PGD A 1
C21 C 0.41484(13) 0.42162(11) 0.31034(7) 0.0513(8) Uani 0.888(3) 1 d PG A 1
H21 H 0.4337 0.4707 0.3250 0.062 Uiso 0.888(3) 1 calc PR A 1
C22 C 0.36302(16) 0.34953(15) 0.32999(6) 0.0717(11) Uani 0.888(3) 1 d PG A 1
H22 H 0.3465 0.3494 0.3581 0.086 Uiso 0.888(3) 1 calc PR A 1
C23 C 0.33535(17) 0.27769(11) 0.30849(9) 0.0662(11) Uani 0.888(3) 1 d PG A 1
H23 H 0.2999 0.2284 0.3219 0.079 Uiso 0.888(3) 1 calc PR A 1
C24 C 0.35951(17) 0.27795(9) 0.26733(9) 0.0620(10) Uani 0.888(3) 1 d PG A 1
H24 H 0.3406 0.2288 0.2526 0.074 Uiso 0.888(3) 1 calc PR A 1
C25 C 0.41133(13) 0.35004(12) 0.24768(6) 0.0469(8) Uani 0.888(3) 1 d PG A 1
H25 H 0.4278 0.3502 0.2196 0.056 Uiso 0.888(3) 1 calc PR A 1
C26 C 0.49556(18) 0.50020(19) 0.24797(11) 0.0503(8) Uani 0.888(3) 1 d PD A 1
H26A H 0.5064 0.4898 0.2193 0.076 Uiso 0.888(3) 1 calc PR A 1
H26B H 0.5459 0.5275 0.2638 0.076 Uiso 0.888(3) 1 calc PR A 1
H26C H 0.4711 0.5342 0.2470 0.076 Uiso 0.888(3) 1 calc PR A 1
C20A C 0.4359(9) 0.3992(8) 0.2428(6) 0.0390(8) Uani 0.112(3) 1 d PGD A 2
C21A C 0.4317(12) 0.4216(9) 0.2838(6) 0.0513(8) Uani 0.112(3) 1 d PGD A 2
H21A H 0.4585 0.4767 0.2913 0.062 Uiso 0.112(3) 1 calc PR A 2
C22A C 0.3884(15) 0.3634(13) 0.3138(6) 0.0717(11) Uani 0.112(3) 1 d PG A 2
H22A H 0.3855 0.3787 0.3418 0.086 Uiso 0.112(3) 1 calc PR A 2
C23A C 0.3492(16) 0.2828(12) 0.3028(8) 0.0662(11) Uani 0.112(3) 1 d PG A 2
H23A H 0.3195 0.2430 0.3233 0.079 Uiso 0.112(3) 1 calc PR A 2
C24A C 0.3533(16) 0.2604(8) 0.2618(9) 0.0620(10) Uani 0.112(3) 1 d PG A 2
H24A H 0.3265 0.2054 0.2543 0.074 Uiso 0.112(3) 1 calc PR A 2
C25A C 0.3967(12) 0.3186(9) 0.2318(7) 0.0469(8) Uani 0.112(3) 1 d PGD A 2
H25A H 0.3995 0.3034 0.2038 0.056 Uiso 0.112(3) 1 calc PR A 2
C26A C 0.4632(14) 0.4642(12) 0.2088(7) 0.0503(8) Uani 0.112(3) 1 d PD A 2
H26D H 0.4712 0.4434 0.1822 0.076 Uiso 0.112(3) 1 calc PR A 2
H26E H 0.5136 0.5112 0.2174 0.076 Uiso 0.112(3) 1 calc PR A 2
H26F H 0.4221 0.4795 0.2050 0.076 Uiso 0.112(3) 1 calc PR A 2
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'
N N 0.0061 0.0033 '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
C7 P1 C1 106.91(9) . .
C7 P1 C13 105.50(8) . .
C1 P1 C13 105.32(9) . .
C7 P1 S1 112.97(6) . .
C1 P1 S1 113.22(7) . .
C13 P1 S1 112.29(6) . .
C19 N1 C19 115.06(17) . 2_575
C6 C1 C2 119.48(19) . .
C6 C1 P1 118.87(17) . .
C2 C1 P1 121.64(15) . .
C3 C2 C1 120.1(2) . .
C3 C2 H2 119.9 . .
C1 C2 H2 119.9 . .
C2 C3 C4 120.2(2) . .
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 . .
C5 C4 C3 119.8(2) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C4 C5 C6 120.6(2) . .
C4 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C1 C6 C5 119.7(2) . .
C1 C6 H6 120.1 . .
C5 C6 H6 120.1 . .
C8 C7 C12 119.51(17) . .
C8 C7 P1 119.67(15) . .
C12 C7 P1 120.41(14) . .
C9 C8 C7 120.38(18) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C9 C10 120.16(19) . .
C8 C9 H9 119.9 . .
C10 C9 H9 119.9 . .
C11 C10 C9 119.95(19) . .
C11 C10 H10 120.0 . .
C9 C10 H10 120.0 . .
C10 C11 C12 120.13(19) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
C7 C12 C11 119.86(18) . .
C7 C12 H12 120.1 . .
C11 C12 H12 120.1 . .
C14 C13 C18 119.59(16) . .
C14 C13 P1 121.76(14) . .
C18 C13 P1 118.65(13) . .
C15 C14 C13 120.26(17) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C14 C15 C16 120.27(17) . .
C14 C15 H15 119.9 . .
C16 C15 H15 119.9 . .
C17 C16 C15 119.19(16) . .
C17 C16 C19 120.41(16) . .
C15 C16 C19 120.38(16) . .
C18 C17 C16 120.77(16) . .
C18 C17 H17 119.6 . .
C16 C17 H17 119.6 . .
C17 C18 C13 119.90(16) . .
C17 C18 H18 120.0 . .
C13 C18 H18 120.0 . .
N1 C19 N1 124.94(16) . 3_355
N1 C19 C16 117.81(15) . .
N1 C19 C16 117.25(15) 3_355 .
C21 C20 C25 120.0 . .
C21 C20 C26 119.92(19) . .
C25 C20 C26 120.08(19) . .
C20 C21 C22 120.0 . .
C20 C21 H21 120.0 . .
C22 C21 H21 120.0 . .
C23 C22 C21 120.0 . .
C23 C22 H22 120.0 . .
C21 C22 H22 120.0 . .
C22 C23 C24 120.0 . .
C22 C23 H23 120.0 . .
C24 C23 H23 120.0 . .
C25 C24 C23 120.0 . .
C25 C24 H24 120.0 . .
C23 C24 H24 120.0 . .
C24 C25 C20 120.0 . .
C24 C25 H25 120.0 . .
C20 C25 H25 120.0 . .
C20 C26 H26A 109.5 . .
C20 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C20 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C21A C20A C25A 120.0 . .
C21A C20A C26A 117.3(8) . .
C25A C20A C26A 120.4(8) . .
C20A C21A C22A 120.0 . .
C20A C21A H21A 120.0 . .
C22A C21A H21A 120.0 . .
C23A C22A C21A 120.0 . .
C23A C22A H22A 120.0 . .
C21A C22A H22A 120.0 . .
C24A C23A C22A 120.0 . .
C24A C23A H23A 120.0 . .
C22A C23A H23A 120.0 . .
C23A C24A C25A 120.0 . .
C23A C24A H24A 120.0 . .
C25A C24A H24A 120.0 . .
C24A C25A C20A 120.0 . .
C24A C25A H25A 120.0 . .
C20A C25A H25A 120.0 . .
C20A C26A H26D 109.5 . .
C20A C26A H26E 109.5 . .
H26D C26A H26E 109.5 . .
C20A C26A H26F 109.5 . .
H26D C26A H26F 109.5 . .
H26E C26A H26F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 P1 1.9505(9) .
P1 C7 1.8116(19) .
P1 C1 1.818(2) .
P1 C13 1.8249(19) .
N1 C19 1.336(2) .
N1 C19 1.343(2) 2_575
C1 C6 1.390(3) .
C1 C2 1.393(3) .
C2 C3 1.384(3) .
C2 H2 0.9500 .
C3 C4 1.388(3) .
C3 H3 0.9500 .
C4 C5 1.373(4) .
C4 H4 0.9500 .
C5 C6 1.392(3) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.394(3) .
C7 C12 1.395(3) .
C8 C9 1.382(3) .
C8 H8 0.9500 .
C9 C10 1.390(3) .
C9 H9 0.9500 .
C10 C11 1.385(3) .
C10 H10 0.9500 .
C11 C12 1.396(3) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.394(3) .
C13 C18 1.400(3) .
C14 C15 1.385(3) .
C14 H14 0.9500 .
C15 C16 1.404(2) .
C15 H15 0.9500 .
C16 C17 1.390(2) .
C16 C19 1.477(2) .
C17 C18 1.386(2) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 N1 1.343(2) 3_355
C20 C21 1.3900 .
C20 C25 1.3900 .
C20 C26 1.509(3) .
C21 C22 1.3900 .
C21 H21 0.9500 .
C22 C23 1.3900 .
C22 H22 0.9500 .
C23 C24 1.3900 .
C23 H23 0.9500 .
C24 C25 1.3900 .
C24 H24 0.9500 .
C25 H25 0.9500 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C20A C21A 1.3900 .
C20A C25A 1.3900 .
C20A C26A 1.537(17) .
C21A C22A 1.3900 .
C21A H21A 0.9500 .
C22A C23A 1.3900 .
C22A H22A 0.9500 .
C23A C24A 1.3900 .
C23A H23A 0.9500 .
C24A C25A 1.3900 .
C24A H24A 0.9500 .
C25A H25A 0.9500 .
C26A H26D 0.9800 .
C26A H26E 0.9800 .
C26A H26F 0.9800 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 186 51 ' '
2 0.000 0.000 0.199 7 0 ' '
3 0.000 0.000 0.801 7 0 ' '
4 0.333 0.667 0.667 190 51 ' '
5 0.333 0.667 0.468 6 0 ' '
6 0.333 0.667 0.865 7 0 ' '
7 0.667 0.333 0.333 190 51 ' '
8 0.667 0.333 0.135 7 0 ' '
9 0.667 0.333 0.532 6 0 ' '
