#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:31:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179505 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/02/4340252.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_4340252
loop_
_publ_author_name
'Cotton, F. Albert'
'Donahue, James P.'
'Gruhn, Nadine E.'
'Lichtenberger, Dennis L.'
'Murillo, Carlos A.'
'Timmons, Daren J.'
'Van Dorn, Laura O.'
'Villagrán, Dino'
'Wang, Xiaoping'
_publ_section_title
;
 Facilitating access to the most easily ionized molecule: an improved
 synthesis of the key intermediate, W2(hpp)4Cl2, and related compounds.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              201
_journal_page_last               213
_journal_paper_doi               10.1021/ic0515709
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C18 H26 N6 O4 W'
_chemical_formula_sum            'C18 H26 N6 O4 W'
_chemical_formula_weight         574.30
_chemical_name_systematic
;
 Tungsten(0) bis(1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidinate)
 tetra(carbonyl)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 91.280(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0954(9)
_cell_length_b                   14.7876(17)
_cell_length_c                   17.043(2)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5425
_cell_measurement_theta_min      2.3905
_cell_volume                     2039.7(4)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL V. 5.03 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_device_type  'area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13983
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.82
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    5.701
_exptl_absorpt_correction_T_max  0.5089
_exptl_absorpt_correction_T_min  0.3878
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         4652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0149
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0193P)²+0.6187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0364
_reflns_number_gt                4221
_reflns_number_total             4652
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic0515709si20050914_104451.cif
_cod_data_source_block           cmpd1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (16
times).

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (16
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (39
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according
to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (12
times).

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4340252
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
W1 W 0.319604(9) 0.227592(5) 0.224073(4) 0.01789(3) Uani 1 1 d
O1 O 0.4017(2) 0.40609(11) 0.32035(10) 0.0397(4) Uani 1 1 d
O2 O 0.5986(2) 0.13244(13) 0.32214(11) 0.0471(5) Uani 1 1 d
O3 O 0.3802(2) 0.05617(12) 0.11641(11) 0.0469(5) Uani 1 1 d
O4 O 0.6013(2) 0.31188(12) 0.12675(12) 0.0446(5) Uani 1 1 d
N1 N 0.1131(2) 0.17237(10) 0.30021(10) 0.0206(3) Uani 1 1 d
N2 N -0.0215(2) 0.30844(12) 0.31060(12) 0.0272(4) Uani 1 1 d
H2A H 0.015(3) 0.3170(16) 0.2635(15) 0.028(6) Uiso 1 1 d
N3 N -0.0714(2) 0.19787(11) 0.40394(10) 0.0230(4) Uani 1 1 d
N4 N 0.1076(2) 0.28629(10) 0.14973(10) 0.0200(3) Uani 1 1 d
N5 N -0.0279(2) 0.15078(12) 0.13462(12) 0.0279(4) Uani 1 1 d
H5A H 0.003(3) 0.1427(16) 0.1785(14) 0.025(6) Uiso 1 1 d
N6 N -0.0815(2) 0.26375(11) 0.04338(11) 0.0220(4) Uani 1 1 d
C1 C 0.3569(3) 0.34172(14) 0.28776(12) 0.0245(4) Uani 1 1 d
C2 C 0.4930(3) 0.16978(14) 0.28709(13) 0.0265(4) Uani 1 1 d
C3 C 0.3423(3) 0.11654(14) 0.15531(13) 0.0264(4) Uani 1 1 d
C4 C 0.4935(3) 0.27923(13) 0.16139(13) 0.0259(5) Uani 1 1 d
C5 C 0.0067(3) 0.22365(12) 0.33790(12) 0.0195(4) Uani 1 1 d
C6 C 0.1392(3) 0.08035(13) 0.33049(13) 0.0231(4) Uani 1 1 d
H6A H 0.226(3) 0.0791(15) 0.3711(14) 0.023(6) Uiso 1 1 d
H6B H 0.177(3) 0.0452(18) 0.2869(14) 0.028(6) Uiso 1 1 d
C7 C -0.0175(3) 0.04210(14) 0.36446(14) 0.0277(5) Uani 1 1 d
H7A H -0.002(3) -0.0174(16) 0.3858(13) 0.023(6) Uiso 1 1 d
H7B H -0.097(3) 0.0383(16) 0.3261(15) 0.032(7) Uiso 1 1 d
C8 C -0.0738(3) 0.10369(15) 0.42912(14) 0.0276(5) Uani 1 1 d
H8B H -0.184(3) 0.0876(15) 0.4448(13) 0.024(6) Uiso 1 1 d
H8A H -0.008(3) 0.0969(16) 0.4770(14) 0.032(7) Uiso 1 1 d
C9 C -0.1823(3) 0.25817(16) 0.44710(16) 0.0306(5) Uani 1 1 d
H9A H -0.165(3) 0.2478(17) 0.5025(18) 0.033(7) Uiso 1 1 d
H9B H -0.292(4) 0.2406(18) 0.4382(17) 0.042(8) Uiso 1 1 d
C10 C -0.1588(3) 0.35634(16) 0.42575(15) 0.0339(5) Uani 1 1 d
H10A H -0.062(3) 0.3811(17) 0.4495(15) 0.037(7) Uiso 1 1 d
H10B H -0.248(3) 0.3942(18) 0.4488(15) 0.040(7) Uiso 1 1 d
C11 C -0.1549(3) 0.36494(16) 0.33776(15) 0.0326(5) Uani 1 1 d
H11B H -0.261(3) 0.3446(15) 0.3146(13) 0.023(6) Uiso 1 1 d
H11A H -0.129(3) 0.4249(18) 0.3214(15) 0.042(7) Uiso 1 1 d
C12 C -0.0009(3) 0.23620(13) 0.10912(12) 0.0196(4) Uani 1 1 d
C13 C 0.1272(3) 0.38032(14) 0.12306(14) 0.0251(4) Uani 1 1 d
H13A H 0.168(3) 0.4153(16) 0.1656(14) 0.028(6) Uiso 1 1 d
H13B H 0.212(3) 0.3829(16) 0.0838(14) 0.030(6) Uiso 1 1 d
C14 C -0.0333(3) 0.41788(14) 0.08977(14) 0.0269(5) Uani 1 1 d
H14A H -0.110(3) 0.4167(16) 0.1297(14) 0.027(6) Uiso 1 1 d
H14B H -0.016(3) 0.4816(15) 0.0700(13) 0.024(6) Uiso 1 1 d
C15 C -0.0896(3) 0.35952(14) 0.02207(13) 0.0265(5) Uani 1 1 d
H15B H -0.019(3) 0.3662(15) -0.0248(13) 0.023(6) Uiso 1 1 d
H15A H -0.201(3) 0.3731(17) 0.0066(15) 0.037(7) Uiso 1 1 d
C16 C -0.1940(3) 0.20513(16) -0.00226(15) 0.0298(5) Uani 1 1 d
H16A H -0.306(4) 0.2221(17) 0.0098(17) 0.042(8) Uiso 1 1 d
H16B H -0.174(4) 0.2208(17) -0.052(2) 0.044(9) Uiso 1 1 d
C17 C -0.1620(3) 0.10660(16) 0.01449(15) 0.0350(5) Uani 1 1 d
H17B H -0.059(4) 0.0890(19) -0.0050(17) 0.049(8) Uiso 1 1 d
H17A H -0.248(4) 0.0709(19) -0.0101(17) 0.049(8) Uiso 1 1 d
C18 C -0.1553(3) 0.09251(16) 0.10191(15) 0.0329(5) Uani 1 1 d
H18B H -0.124(3) 0.0309(19) 0.1151(15) 0.042(7) Uiso 1 1 d
H18A H -0.264(3) 0.1094(17) 0.1257(15) 0.039(7) Uiso 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'
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_publ_flag
C4 W1 C2 87.34(9) y
C4 W1 C1 82.29(8) y
C2 W1 C1 88.46(9) y
C4 W1 C3 85.66(8) y
C2 W1 C3 83.67(9) y
C1 W1 C3 165.90(9) y
C4 W1 N4 95.20(8) y
C2 W1 N4 176.18(7) y
C1 W1 N4 94.70(7) y
C3 W1 N4 93.66(7) y
C4 W1 N1 177.68(7) y
C2 W1 N1 93.28(8) y
C1 W1 N1 95.49(7) y
C3 W1 N1 96.63(7) y
N4 W1 N1 84.30(6) y
C5 N1 C6 116.75(17) y
C5 N1 W1 124.16(12) y
C6 N1 W1 115.37(12) y
C5 N2 C11 123.03(18) y
C5 N3 C8 121.45(17) y
C5 N3 C9 122.96(18) y
C8 N3 C9 114.77(17) y
C12 N4 C13 116.07(17) y
C12 N4 W1 123.81(13) y
C13 N4 W1 116.46(13) y
C12 N5 C18 123.4(2) y
C12 N6 C15 121.16(18) y
C12 N6 C16 123.06(17) y
C15 N6 C16 114.60(18) y
O1 C1 W1 169.99(19) y
O2 C2 W1 176.9(2) y
O3 C3 W1 169.74(19) y
O4 C4 W1 176.9(2) y
N1 C5 N2 118.03(18) y
N1 C5 N3 124.14(17) y
N2 C5 N3 117.78(18) y
N1 C6 C7 111.41(17) n
C8 C7 C6 108.85(18) n
N3 C8 C7 110.84(18) n
N3 C9 C10 112.35(19) n
C11 C10 C9 109.1(2) n
N2 C11 C10 107.5(2) n
N4 C12 N6 124.46(17) y
N4 C12 N5 117.46(19) y
N6 C12 N5 118.04(19) y
N4 C13 C14 111.42(17) n
C15 C14 C13 108.71(18) n
N6 C15 C14 110.73(18) n
N6 C16 C17 111.64(19) n
C18 C17 C16 108.9(2) n
N5 C18 C17 108.0(2) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
W1 C4 1.943(2) y
W1 C2 1.946(2) y
W1 C1 2.026(2) y
W1 C3 2.028(2) y
W1 N4 2.2821(17) y
W1 N1 2.2896(16) y
O1 C1 1.156(3) y
O2 C2 1.170(3) y
O3 C3 1.158(3) y
O4 C4 1.169(3) y
N1 C5 1.324(2) y
N1 C6 1.469(2) n
N2 C5 1.355(3) y
N2 C11 1.449(3) n
N3 C5 1.358(3) y
N3 C8 1.458(3) n
N3 C9 1.473(3) n
N4 C12 1.331(3) y
N4 C13 1.473(2) n
N5 C12 1.355(3) y
N5 C18 1.446(3) n
N6 C12 1.347(3) y
N6 C15 1.463(3) n
N6 C16 1.468(3) n
C6 C7 1.515(3) n
C7 C8 1.508(3) n
C9 C10 1.510(3) n
C10 C11 1.506(4) n
C13 C14 1.512(3) n
C14 C15 1.504(3) n
C16 C17 1.506(3) n
C17 C18 1.504(4) n
