#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/29/7012919.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_7012919
loop_
_publ_author_name
'Grundy, Joanna'
'Coles, Martyn P.'
'Hitchcock, Peter B.'
_publ_section_title
;
 Synthesis and coordination chemistry of neutral
 phospha(iii)guanidines. Formation of
 1-aza-3-phospha-4-metallacyclobut-1-ene rings at group 6
 metalsElectronic supplementary information (ESI) available: an ORTEP
 representation and bond lengths and angles for 3a; crystal structure
 and refinement data, bond lengths and angles and an ORTEP
 representation of the molecular structure of Mo(CO)4(pip)2. See
 http://www.rsc.org/suppdata/dt/b3/b302554c/
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              2573
_journal_paper_doi               10.1039/b302554c
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29 H33 N2 O4 P1 W1'
_chemical_formula_sum            'C29 H33 N2 O4 P W'
_chemical_formula_weight         688.39
_chemical_name_common            '[W(CO)4{PPh2C(Ncy)(NHcy)}]'
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-10-19T11:20:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 118.084(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.0487(3)
_cell_length_b                   9.4740(1)
_cell_length_c                   21.3526(3)
_cell_measurement_reflns_used    17518
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     5719.93(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.031
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25963
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    4.131
_exptl_absorpt_correction_T_max  0.6653
_exptl_absorpt_correction_T_min  0.3998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.636
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    'H on N2 refined; others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0218P)²+9.5727P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                6127
_reflns_number_total             6797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302554c.txt
_cod_data_source_block           mpc-3a(oct1602)
_cod_original_cell_volume        5719.92(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C29 H33 N2 O4 P1 W1'
_cod_database_code               7012919
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
W W 0.148956(3) 0.851330(9) 0.019179(5) 0.02158(4) Uani 1 1 d . . .
P P 0.12834(2) 0.76216(6) 0.11092(3) 0.02083(12) Uani 1 1 d . . .
O1 O 0.04829(9) 0.8578(3) -0.11630(15) 0.0630(8) Uani 1 1 d . . .
O2 O 0.25759(8) 0.8438(2) 0.13507(14) 0.0523(6) Uani 1 1 d . . .
O3 O 0.18350(9) 0.9158(3) -0.09280(13) 0.0649(7) Uani 1 1 d . . .
O4 O 0.13765(8) 1.17185(19) 0.03951(12) 0.0453(5) Uani 1 1 d . . .
N1 N 0.14453(7) 0.6108(2) 0.02876(10) 0.0220(4) Uani 1 1 d . . .
N2 N 0.11877(8) 0.4602(2) 0.09289(12) 0.0316(5) Uani 1 1 d . . .
H2 H 0.1203(11) 0.390(4) 0.0712(18) 0.042(9) Uiso 1 1 d . . .
C1 C 0.08332(10) 0.8523(3) -0.06535(16) 0.0336(6) Uani 1 1 d . . .
C2 C 0.21862(10) 0.8461(3) 0.09475(15) 0.0299(5) Uani 1 1 d . . .
C3 C 0.17113(10) 0.8895(3) -0.05195(16) 0.0363(6) Uani 1 1 d . . .
C4 C 0.14334(9) 1.0518(3) 0.03101(13) 0.0284(5) Uani 1 1 d . . .
C5 C 0.13013(8) 0.5852(2) 0.07534(12) 0.0219(4) Uani 1 1 d . . .
C6 C 0.17503(8) 0.7687(2) 0.20184(12) 0.0224(4) Uani 1 1 d . . .
C7 C 0.18188(10) 0.8966(3) 0.23824(14) 0.0319(5) Uani 1 1 d . . .
H7 H 0.1604 0.9711 0.2171 0.038 Uiso 1 1 calc R . .
C8 C 0.21983(10) 0.9145(3) 0.30468(15) 0.0372(6) Uani 1 1 d . . .
H8 H 0.2238 1.0002 0.329 0.045 Uiso 1 1 calc R . .
C9 C 0.25204(10) 0.8067(3) 0.33553(15) 0.0384(6) Uani 1 1 d . . .
H9 H 0.2779 0.8191 0.3809 0.046 Uiso 1 1 calc R . .
C10 C 0.24633(9) 0.6805(3) 0.29994(16) 0.0364(6) Uani 1 1 d . . .
H10 H 0.2687 0.6079 0.3208 0.044 Uiso 1 1 calc R . .
C11 C 0.20782(9) 0.6606(3) 0.23358(15) 0.0298(5) Uani 1 1 d . . .
H11 H 0.2038 0.574 0.2099 0.036 Uiso 1 1 calc R . .
C12 C 0.07339(8) 0.7871(2) 0.11513(14) 0.0266(5) Uani 1 1 d . . .
C13 C 0.03289(10) 0.8172(3) 0.05240(17) 0.0405(6) Uani 1 1 d . . .
H13 H 0.0346 0.8253 0.0098 0.049 Uiso 1 1 calc R . .
C14 C -0.01016(11) 0.8355(4) 0.0522(2) 0.0524(9) Uani 1 1 d . . .
H14 H -0.0376 0.8541 0.0094 0.063 Uiso 1 1 calc R . .
C15 C -0.01260(12) 0.8263(3) 0.1144(2) 0.0532(9) Uani 1 1 d . . .
H15 H -0.0417 0.8388 0.1143 0.064 Uiso 1 1 calc R . .
C16 C 0.02746(12) 0.7989(4) 0.1771(2) 0.0541(9) Uani 1 1 d . . .
H16 H 0.0257 0.7937 0.2197 0.065 Uiso 1 1 calc R . .
C17 C 0.07046(10) 0.7788(3) 0.17760(16) 0.0392(6) Uani 1 1 d . . .
H17 H 0.0977 0.7594 0.2205 0.047 Uiso 1 1 calc R . .
C18 C 0.15127(8) 0.4949(2) -0.01166(13) 0.0239(5) Uani 1 1 d . . .
H18 H 0.1545 0.406 0.0146 0.029 Uiso 1 1 calc R . .
C19 C 0.19605(9) 0.5154(3) -0.01784(15) 0.0324(6) Uani 1 1 d . . .
H19A H 0.2232 0.5233 0.0296 0.039 Uiso 1 1 calc R . .
H19B H 0.1938 0.603 -0.0437 0.039 Uiso 1 1 calc R . .
C20 C 0.20323(10) 0.3903(3) -0.05722(16) 0.0364(6) Uani 1 1 d . . .
H20A H 0.2318 0.4056 -0.062 0.044 Uiso 1 1 calc R . .
H20B H 0.2077 0.3039 -0.0295 0.044 Uiso 1 1 calc R . .
C21 C 0.16106(12) 0.3722(3) -0.13046(17) 0.0416(7) Uani 1 1 d . . .
H21A H 0.1656 0.2878 -0.1531 0.05 Uiso 1 1 calc R . .
H21B H 0.1588 0.4539 -0.16 0.05 Uiso 1 1 calc R . .
C22 C 0.11539(11) 0.3579(3) -0.12521(18) 0.0460(8) Uani 1 1 d . . .
H22A H 0.1161 0.2691 -0.1012 0.055 Uiso 1 1 calc R . .
H22B H 0.0885 0.3543 -0.1731 0.055 Uiso 1 1 calc R . .
C23 C 0.10849(9) 0.4807(3) -0.08442(15) 0.0378(6) Uani 1 1 d . . .
H23A H 0.104 0.5685 -0.1111 0.045 Uiso 1 1 calc R . .
H23B H 0.0801 0.4643 -0.0791 0.045 Uiso 1 1 calc R . .
C24 C 0.10541(9) 0.4329(2) 0.14852(13) 0.0273(5) Uani 1 1 d . . .
H24 H 0.1163 0.5134 0.182 0.033 Uiso 1 1 calc R . .
C25 C 0.05203(10) 0.4180(3) 0.11898(17) 0.0404(7) Uani 1 1 d . . .
H25A H 0.0365 0.5059 0.0953 0.049 Uiso 1 1 calc R . .
H25B H 0.0404 0.3421 0.0837 0.049 Uiso 1 1 calc R . .
C26 C 0.03939(13) 0.3853(4) 0.1777(2) 0.0556(9) Uani 1 1 d . . .
H26A H 0.005 0.3746 0.1573 0.067 Uiso 1 1 calc R . .
H26B H 0.0492 0.464 0.2114 0.067 Uiso 1 1 calc R . .
C27 C 0.06358(14) 0.2506(4) 0.2166(2) 0.0606(10) Uani 1 1 d . . .
H27A H 0.056 0.2336 0.2555 0.073 Uiso 1 1 calc R . .
H27B H 0.0517 0.1704 0.1839 0.073 Uiso 1 1 calc R . .
C28 C 0.11664(13) 0.2617(3) 0.24624(18) 0.0489(8) Uani 1 1 d . . .
H28A H 0.1312 0.1714 0.2679 0.059 Uiso 1 1 calc R . .
H28B H 0.1288 0.334 0.2835 0.059 Uiso 1 1 calc R . .
C29 C 0.13056(11) 0.2996(3) 0.18919(16) 0.0371(6) Uani 1 1 d . . .
H29A H 0.1226 0.2207 0.1558 0.045 Uiso 1 1 calc R . .
H29B H 0.1648 0.3141 0.2114 0.045 Uiso 1 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 0 '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 0.006 '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 -0.849 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
_geom_angle_publ_flag
C4 W C3 90.57(11) . . ?
C4 W C1 89.46(10) . . ?
C3 W C1 85.03(12) . . ?
C4 W C2 93.14(10) . . ?
C3 W C2 87.55(11) . . ?
C1 W C2 172.16(11) . . ?
C4 W N1 161.42(9) . . ?
C3 W N1 107.89(10) . . ?
C1 W N1 90.11(8) . . ?
C2 W N1 89.77(8) . . ?
C4 W P 98.90(8) . . ?
C3 W P 169.77(9) . . ?
C1 W P 98.82(9) . . ?
C2 W P 88.09(8) . . ?
N1 W P 62.84(5) . . ?
C6 P C12 105.85(11) . . ?
C6 P C5 107.52(10) . . ?
C12 P C5 110.80(10) . . ?
C6 P W 116.13(7) . . ?
C12 P W 128.00(8) . . ?
C5 P W 85.04(7) . . ?
C5 N1 C18 120.75(19) . . ?
C5 N1 W 108.17(15) . . ?
C18 N1 W 130.86(15) . . ?
C5 N2 C24 127.1(2) . . ?
O1 C1 W 173.8(3) . . ?
O2 C2 W 178.0(3) . . ?
O3 C3 W 177.8(3) . . ?
O4 C4 W 175.6(2) . . ?
N1 C5 N2 128.2(2) . . ?
N1 C5 P 103.61(16) . . ?
N2 C5 P 128.22(18) . . ?
C11 C6 C7 118.8(2) . . ?
C11 C6 P 123.36(18) . . ?
C7 C6 P 117.33(18) . . ?
C8 C7 C6 120.6(3) . . ?
C7 C8 C9 120.1(3) . . ?
C8 C9 C10 120.1(3) . . ?
C9 C10 C11 120.3(3) . . ?
C10 C11 C6 120.1(2) . . ?
C17 C12 C13 119.1(2) . . ?
C17 C12 P 123.1(2) . . ?
C13 C12 P 117.8(2) . . ?
C12 C13 C14 120.4(3) . . ?
C15 C14 C13 120.0(3) . . ?
C14 C15 C16 120.2(3) . . ?
C15 C16 C17 120.2(3) . . ?
C12 C17 C16 120.2(3) . . ?
N1 C18 C19 111.20(19) . . ?
N1 C18 C23 110.76(19) . . ?
C19 C18 C23 111.0(2) . . ?
C18 C19 C20 110.0(2) . . ?
C21 C20 C19 111.2(2) . . ?
C20 C21 C22 110.7(2) . . ?
C21 C22 C23 112.0(2) . . ?
C18 C23 C22 110.3(2) . . ?
N2 C24 C25 112.4(2) . . ?
N2 C24 C29 109.2(2) . . ?
C25 C24 C29 110.3(2) . . ?
C26 C25 C24 111.1(3) . . ?
C25 C26 C27 110.9(3) . . ?
C28 C27 C26 110.7(3) . . ?
C27 C28 C29 112.1(3) . . ?
C28 C29 C24 111.9(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
W C4 1.936(3) . ?
W C3 1.990(3) . ?
W C1 2.027(3) . ?
W C2 2.049(3) . ?
W N1 2.299(2) . ?
W P 2.4913(6) . ?
P C6 1.810(2) . ?
P C12 1.821(2) . ?
P C5 1.853(2) . ?
O1 C1 1.139(4) . ?
O2 C2 1.135(3) . ?
O3 C3 1.143(3) . ?
O4 C4 1.179(3) . ?
N1 C5 1.301(3) . ?
N1 C18 1.474(3) . ?
N2 C5 1.343(3) . ?
N2 C24 1.463(3) . ?
C6 C11 1.393(3) . ?
C6 C7 1.400(3) . ?
C7 C8 1.377(4) . ?
C8 C9 1.379(4) . ?
C9 C10 1.382(4) . ?
C10 C11 1.386(4) . ?
C12 C17 1.383(4) . ?
C12 C13 1.387(4) . ?
C13 C14 1.388(4) . ?
C14 C15 1.370(5) . ?
C15 C16 1.374(5) . ?
C16 C17 1.386(4) . ?
C18 C19 1.514(3) . ?
C18 C23 1.519(3) . ?
C19 C20 1.532(4) . ?
C20 C21 1.520(4) . ?
C21 C22 1.526(4) . ?
C22 C23 1.531(4) . ?
C24 C25 1.526(4) . ?
C24 C29 1.530(4) . ?
C25 C26 1.521(5) . ?
C26 C27 1.521(5) . ?
C27 C28 1.513(5) . ?
C28 C29 1.524(4) . ?
