#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:49:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179991 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/85/7028593.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_7028593
loop_
_publ_author_name
'Naik, Susmita'
'Kumaravel, Maruthai'
'Mague, Joel T.'
'Balakrishna, Maravanji S.'
_publ_section_title
;
 Bisamino(diphosphonite) with dangling olefin functionalities: synthesis,
 metal chemistry and catalytic utility of Rh(I) and Pd(II) complexes in
 hydroformylation and Suzuki-Miyaura reactions.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1082
_journal_page_last               1095
_journal_paper_doi               10.1039/c3dt52400k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C43 H38 N O8 P2 W'
_chemical_formula_sum            'C43 H38 N O8 P2 W'
_chemical_formula_weight         945.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.0377(17)
_cell_length_b                   21.0377(17)
_cell_length_c                   17.7433(15)
_cell_measurement_reflns_used    9698
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      2.45
_cell_volume                     7852.9(11)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2009a)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2009a)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-I 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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70156
_diffrn_reflns_theta_full        29.17
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    3.078
_exptl_absorpt_correction_T_max  0.7127
_exptl_absorpt_correction_T_min  0.4650
_exptl_absorpt_correction_type   'integration numerical Gaussian'
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5271
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0259P)²+24.1691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                4445
_reflns_number_total             5271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52400k.txt
_cod_data_source_block           msb423_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/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      I4(1)/a
_cod_database_code               7028593
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
W1 W 0.5000 0.2500 0.037758(7) 0.02921(5) Uani 1 2 d S . .
P1 P 0.44997(3) 0.21344(3) 0.15368(3) 0.02440(13) Uani 1 1 d . . .
O1 O 0.44341(8) 0.14018(8) 0.17994(10) 0.0263(4) Uani 1 1 d . . .
O2 O 0.38289(8) 0.23646(9) 0.18824(10) 0.0285(4) Uani 1 1 d . . .
O3 O 0.40559(12) 0.36627(10) 0.01452(12) 0.0454(5) Uani 1 1 d . . .
O4 O 0.58553(12) 0.32190(11) -0.08092(12) 0.0481(6) Uani 1 1 d . . .
N1 N 0.5000 0.2500 0.21497(14) 0.0203(5) Uani 1 2 d S . .
C1 C 0.48597(13) 0.09210(12) 0.15783(14) 0.0272(5) Uani 1 1 d . A .
C2 C 0.54652(13) 0.09110(13) 0.18815(16) 0.0316(5) Uani 1 1 d . . .
H2 H 0.5608 0.1251 0.2190 0.038 Uiso 1 1 calc R . .
C3 C 0.58615(15) 0.04021(14) 0.17321(17) 0.0379(6) Uani 1 1 d . . .
H3 H 0.6280 0.0392 0.1933 0.046 Uiso 1 1 calc R . .
C4 C 0.56429(17) -0.00940(14) 0.12867(18) 0.0425(7) Uani 1 1 d . . .
H4 H 0.5908 -0.0451 0.1193 0.051 Uiso 1 1 calc R . .
C5 C 0.50389(17) -0.00701(14) 0.09778(18) 0.0413(7) Uani 1 1 d . A .
H5 H 0.4897 -0.0412 0.0670 0.050 Uiso 1 1 calc R . .
C6 C 0.46320(14) 0.04441(13) 0.11073(15) 0.0321(6) Uani 1 1 d . . .
C7 C 0.39676(15) 0.04556(16) 0.07837(16) 0.0429(7) Uani 0.50 1 d PD A 1
H7A H 0.3880 0.0887 0.0587 0.051 Uiso 0.50 1 calc PR A 1
H7B H 0.3949 0.0157 0.0353 0.051 Uiso 0.50 1 calc PR A 1
C8 C 0.3457(3) 0.0282(3) 0.1334(4) 0.0477(12) Uani 0.50 1 d PD A 1
H8 H 0.3337 0.0567 0.1724 0.057 Uiso 0.50 1 calc PR A 1
C9 C 0.3183(5) -0.0269(4) 0.1263(7) 0.078(2) Uani 0.50 1 d PD A 1
H9A H 0.3308 -0.0549 0.0870 0.094 Uiso 0.50 1 calc PR A 1
H9B H 0.2857 -0.0391 0.1604 0.094 Uiso 0.50 1 calc PR A 1
C7A C 0.39676(15) 0.04556(16) 0.07837(16) 0.0429(7) Uani 0.50 1 d PD A 2
H7A1 H 0.3976 0.0352 0.0239 0.051 Uiso 0.50 1 calc PR A 2
H7A2 H 0.3774 0.0881 0.0849 0.051 Uiso 0.50 1 calc PR A 2
C8A C 0.3592(3) -0.0042(3) 0.1216(4) 0.0477(12) Uani 0.50 1 d PD A 2
H8A H 0.3776 -0.0455 0.1220 0.057 Uiso 0.50 1 calc PR A 2
C9A C 0.3062(4) 0.0009(5) 0.1579(6) 0.078(2) Uani 0.50 1 d PD A 2
H9A1 H 0.2849 0.0407 0.1601 0.094 Uiso 0.50 1 calc PR A 2
H9A2 H 0.2885 -0.0351 0.1825 0.094 Uiso 0.50 1 calc PR A 2
C10 C 0.32546(14) 0.21033(13) 0.16187(17) 0.0360(6) Uani 1 1 d . . .
C11 C 0.30981(18) 0.21783(17) 0.0865(2) 0.0521(9) Uani 1 1 d . . .
H11 H 0.3382 0.2384 0.0528 0.062 Uiso 1 1 calc R . .
C12 C 0.2521(2) 0.1948(2) 0.0613(3) 0.0725(15) Uani 1 1 d . . .
H12 H 0.2406 0.1992 0.0098 0.087 Uiso 1 1 calc R . .
C13 C 0.2116(2) 0.1658(2) 0.1104(3) 0.0807(17) Uani 1 1 d . . .
H13 H 0.1718 0.1506 0.0928 0.097 Uiso 1 1 calc R . .
C14 C 0.22767(18) 0.15809(16) 0.1862(3) 0.0628(12) Uani 1 1 d . . .
H14 H 0.1986 0.1381 0.2196 0.075 Uiso 1 1 calc R . .
C15 C 0.28651(14) 0.17968(13) 0.2133(2) 0.0399(7) Uani 1 1 d . . .
C16 C 0.30535(13) 0.17032(14) 0.29450(18) 0.0378(6) Uani 1 1 d . . .
H16A H 0.3520 0.1645 0.2971 0.045 Uiso 1 1 calc R . .
H16B H 0.2947 0.2093 0.3230 0.045 Uiso 1 1 calc R . .
C17 C 0.27381(14) 0.11447(15) 0.3321(2) 0.0444(8) Uani 1 1 d . . .
H17 H 0.2797 0.0738 0.3098 0.053 Uiso 1 1 calc R . .
C18 C 0.23893(17) 0.11743(18) 0.3929(2) 0.0526(9) Uani 1 1 d . . .
H18A H 0.2319 0.1572 0.4169 0.063 Uiso 1 1 calc R . .
H18B H 0.2206 0.0798 0.4132 0.063 Uiso 1 1 calc R . .
C19 C 0.5000 0.2500 0.29610(17) 0.0213(6) Uani 1 2 d S . .
C20 C 0.4823(2) 0.1959(2) 0.3353(3) 0.0232(6) Uani 0.50 1 d P . .
H20 H 0.4700 0.1618 0.3108 0.028 Uiso 0.50 1 d PR . .
C20A C 0.4466(2) 0.2688(2) 0.3363(3) 0.0232(6) Uani 0.50 1 d P . .
H20A H 0.4132 0.2842 0.3076 0.028 Uiso 0.50 1 d PR . .
C21 C 0.43951(16) 0.32547(14) 0.02689(15) 0.0355(6) Uani 1 1 d . . .
C22 C 0.55438(16) 0.29542(14) -0.03873(15) 0.0370(6) 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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
C22 W1 C22 95.37(16) . 6_554
C22 W1 C21 87.21(12) . 6_554
C22 W1 C21 85.50(12) 6_554 6_554
C22 W1 C21 85.50(12) . .
C22 W1 C21 87.21(12) 6_554 .
C21 W1 C21 169.17(15) 6_554 .
C22 W1 P1 100.00(8) . 6_554
C22 W1 P1 164.50(8) 6_554 6_554
C21 W1 P1 93.21(8) 6_554 6_554
C21 W1 P1 95.94(8) . 6_554
C22 W1 P1 164.50(8) . .
C22 W1 P1 100.00(8) 6_554 .
C21 W1 P1 95.94(8) 6_554 .
C21 W1 P1 93.21(8) . .
P1 W1 P1 64.73(3) 6_554 .
O2 P1 O1 95.85(10) . .
O2 P1 N1 99.37(8) . .
O1 P1 N1 107.48(8) . .
O2 P1 W1 127.18(7) . .
O1 P1 W1 125.57(7) . .
N1 P1 W1 97.47(7) . .
C1 O1 P1 123.44(16) . .
C10 O2 P1 120.49(17) . .
C19 N1 P1 129.84(7) . .
C19 N1 P1 129.84(7) . 6_554
P1 N1 P1 100.33(14) . 6_554
C2 C1 C6 122.7(2) . .
C2 C1 O1 119.3(2) . .
C6 C1 O1 117.8(2) . .
C3 C2 C1 119.5(3) . .
C3 C2 H2 120.2 . .
C1 C2 H2 120.2 . .
C2 C3 C4 119.5(3) . .
C2 C3 H3 120.3 . .
C4 C3 H3 120.3 . .
C5 C4 C3 120.1(3) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 121.7(3) . .
C4 C5 H5 119.2 . .
C6 C5 H5 119.2 . .
C1 C6 C5 116.5(3) . .
C1 C6 C7 122.4(3) . .
C5 C6 C7 121.1(3) . .
C8 C7 C6 114.3(4) . .
C8 C7 H7A 108.7 . .
C6 C7 H7A 108.7 . .
C8 C7 H7B 108.7 . .
C6 C7 H7B 108.7 . .
H7A C7 H7B 107.6 . .
C9 C8 C7 118.2(6) . .
C9 C8 H8 120.9 . .
C7 C8 H8 120.9 . .
C8 C9 H9A 120.0 . .
C8 C9 H9B 120.0 . .
H9A C9 H9B 120.0 . .
C9A C8A H8A 115.0 . .
C8A C9A H9A1 120.0 . .
C8A C9A H9A2 120.0 . .
H9A1 C9A H9A2 120.0 . .
C15 C10 C11 123.2(3) . .
C15 C10 O2 118.1(3) . .
C11 C10 O2 118.7(3) . .
C12 C11 C10 118.7(4) . .
C12 C11 H11 120.6 . .
C10 C11 H11 120.6 . .
C13 C12 C11 120.0(4) . .
C13 C12 H12 120.0 . .
C11 C12 H12 120.0 . .
C12 C13 C14 121.1(4) . .
C12 C13 H13 119.4 . .
C14 C13 H13 119.4 . .
C13 C14 C15 120.4(4) . .
C13 C14 H14 119.8 . .
C15 C14 H14 119.8 . .
C10 C15 C14 116.5(3) . .
C10 C15 C16 122.3(3) . .
C14 C15 C16 121.1(3) . .
C17 C16 C15 114.2(3) . .
C17 C16 H16A 108.7 . .
C15 C16 H16A 108.7 . .
C17 C16 H16B 108.7 . .
C15 C16 H16B 108.7 . .
H16A C16 H16B 107.6 . .
C18 C17 C16 125.2(3) . .
C18 C17 H17 117.4 . .
C16 C17 H17 117.4 . .
C17 C18 H18A 120.0 . .
C17 C18 H18B 120.0 . .
H18A C18 H18B 120.0 . .
C20 C19 C20 119.7(4) . 6_554
C20 C19 C20A 74.1(3) . 6_554
C20 C19 C20A 76.0(3) 6_554 6_554
C20 C19 C20A 76.0(3) . .
C20 C19 C20A 74.1(3) 6_554 .
C20A C19 C20A 118.2(4) 6_554 .
C20 C19 N1 120.2(2) . .
C20 C19 N1 120.2(2) 6_554 .
C20A C19 N1 120.9(2) 6_554 .
C20A C19 N1 120.9(2) . .
C19 C20 C20A 119.9(4) . 16_656
C19 C20 C20A 53.1(2) . 6_554
C20A C20 C20A 90.0(4) 16_656 6_554
C19 C20 H20 120.1 . .
C20A C20 H20 119.9 16_656 .
C20A C20 H20 129.2 6_554 .
C19 C20A C20 121.1(4) . 11_666
C19 C20A C20 52.8(2) . 6_554
C20 C20A C20 91.6(4) 11_666 6_554
C19 C20A H20A 115.4 . .
C20 C20A H20A 123.3 11_666 .
C20 C20A H20A 121.2 6_554 .
O3 C21 W1 174.2(2) . .
O4 C22 W1 178.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C22 2.016(3) .
W1 C22 2.016(3) 6_554
W1 C21 2.044(3) 6_554
W1 C21 2.044(3) .
W1 P1 2.4351(7) 6_554
W1 P1 2.4352(7) .
P1 O2 1.6130(19) .
P1 O1 1.6160(18) .
P1 N1 1.6976(18) .
O1 C1 1.407(3) .
O2 C10 1.407(3) .
O3 C21 1.138(4) .
O4 C22 1.140(4) .
N1 C19 1.439(4) .
N1 P1 1.6976(17) 6_554
C1 C2 1.383(4) .
C1 C6 1.391(4) .
C2 C3 1.383(4) .
C2 H2 0.9500 .
C3 C4 1.388(4) .
C3 H3 0.9500 .
C4 C5 1.385(5) .
C4 H4 0.9500 .
C5 C6 1.398(4) .
C5 H5 0.9500 .
C6 C7 1.511(4) .
C7 C8 1.496(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.301(5) .
C8 H8 0.9500 .
C9 H9A 0.9500 .
C9 H9B 0.9500 .
C8A C9A 1.293(5) .
C8A H8A 0.9500 .
C9A H9A1 0.9500 .
C9A H9A2 0.9500 .
C10 C15 1.385(5) .
C10 C11 1.387(4) .
C11 C12 1.381(5) .
C11 H11 0.9500 .
C12 C13 1.362(7) .
C12 H12 0.9500 .
C13 C14 1.396(7) .
C13 H13 0.9500 .
C14 C15 1.403(4) .
C14 H14 0.9500 .
C15 C16 1.508(4) .
C16 C17 1.505(4) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.307(5) .
C17 H17 0.9500 .
C18 H18A 0.9500 .
C18 H18B 0.9500 .
C19 C20 1.385(5) .
C19 C20 1.385(5) 6_554
C19 C20A 1.389(5) 6_554
C19 C20A 1.389(5) .
C20 C20A 1.391(6) 16_656
C20 C20A 1.671(7) 6_554
C20 H20 0.8774 .
C20A C20 1.391(6) 11_666
C20A C20 1.671(7) 6_554
C20A H20A 0.9250 .
