#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:31:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179505 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/02/4340249.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_4340249
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         'C30 H48 N12 O2 W2 , 2(C H2 Cl2)'
_chemical_formula_sum            'C32 H52 Cl4 N12 O2 W2'
_chemical_formula_weight         1146.36
_chemical_name_common            ' W2(μ-hpp)2(η-hpp)2(μ-CO)2,2CH2Cl2'
_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                102.471(2)
_cell_angle_beta                 101.692(2)
_cell_angle_gamma                114.904(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1469(9)
_cell_length_b                   10.8208(10)
_cell_length_c                   11.8963(12)
_cell_measurement_reflns_used    5649
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.507
_cell_measurement_theta_min      2.3535
_cell_volume                     983.81(17)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6946
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.21
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    6.161
_exptl_absorpt_correction_T_max  0.4991
_exptl_absorpt_correction_T_min  0.2299
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.122
_refine_diff_density_min         -1.938
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0272
_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)+(0.0495P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                4076
_reflns_number_total             4344
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic0515709si20050914_104451.cif
_cod_data_source_block           cmpd2TwoCH2Cl2
_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 (25
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 (12
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 (55
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 (19
times).

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4340249
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
W1 W 0.577931(15) 0.614343(14) 0.087459(12) 0.01856(7) Uani 1 1 d . . .
Cl1 Cl 0.70456(19) 0.49099(19) 0.49534(14) 0.0604(4) Uani 1 1 d . . .
Cl2 Cl 0.5605(3) 0.2178(2) 0.2988(2) 0.0945(6) Uani 1 1 d . . .
O1 O 0.2944(3) 0.3629(3) 0.1331(3) 0.0307(6) Uani 1 1 d . . .
N1 N 0.7656(4) 0.5522(4) 0.1455(3) 0.0222(6) Uani 1 1 d . . .
N2 N 0.6006(4) 0.3253(4) -0.0079(3) 0.0225(6) Uani 1 1 d . . .
N3 N 0.8730(4) 0.3842(4) 0.1128(4) 0.0298(8) Uani 1 1 d . . .
N4 N 0.6386(4) 0.7537(4) 0.2687(3) 0.0284(7) Uani 1 1 d . B .
N5 N 0.7835(4) 0.8376(4) 0.1501(3) 0.0256(7) Uani 1 1 d . . .
N6 N 0.8389(5) 1.0056(4) 0.3400(4) 0.0386(9) Uani 1 1 d . B .
C1 C 0.3964(4) 0.4470(4) 0.1018(3) 0.0211(7) Uani 1 1 d . . .
C2 C 0.7480(5) 0.4236(5) 0.0843(4) 0.0224(8) Uani 1 1 d . . .
C3 C 0.9278(5) 0.6558(5) 0.2457(4) 0.0309(9) Uani 1 1 d . . .
H3A H 1.008(6) 0.726(5) 0.211(4) 0.030(12) Uiso 1 1 d . . .
H3B H 0.901(7) 0.724(7) 0.307(6) 0.059(18) Uiso 1 1 d . . .
C4 C 1.0105(6) 0.5819(6) 0.3071(4) 0.0386(11) Uani 1 1 d . . .
H4A H 1.123(8) 0.655(8) 0.360(6) 0.07(2) Uiso 1 1 d . . .
H4B H 0.935(8) 0.538(8) 0.357(6) 0.08(2) Uiso 1 1 d . . .
C5 C 1.0345(6) 0.4828(6) 0.2123(5) 0.0366(10) Uani 1 1 d . . .
H5A H 1.127(7) 0.537(7) 0.176(5) 0.049(16) Uiso 1 1 d . . .
H5B H 1.076(7) 0.424(6) 0.242(5) 0.048(16) Uiso 1 1 d . . .
C6 C 0.8928(6) 0.2861(5) 0.0187(5) 0.0344(10) Uani 1 1 d . . .
H6B H 0.942(6) 0.241(6) 0.055(5) 0.032(13) Uiso 1 1 d . . .
H6A H 0.989(8) 0.345(7) -0.010(6) 0.058(18) Uiso 1 1 d . . .
C7 C 0.7284(6) 0.1837(6) -0.0879(5) 0.0364(10) Uani 1 1 d . . .
H7A H 0.723(5) 0.212(5) -0.156(4) 0.027(11) Uiso 1 1 d . . .
H7B H 0.729(6) 0.094(6) -0.113(5) 0.036(14) Uiso 1 1 d . . .
C8 C 0.5808(5) 0.1797(5) -0.0462(4) 0.0285(8) Uani 1 1 d . . .
H8A H 0.472(7) 0.116(6) -0.111(5) 0.045(15) Uiso 1 1 d . . .
H8B H 0.588(5) 0.148(5) 0.025(4) 0.021(10) Uiso 1 1 d . . .
C9 C 0.7561(5) 0.8701(5) 0.2557(4) 0.0256(8) Uani 1 1 d . . .
C10 C 0.8995(6) 0.9498(5) 0.1145(5) 0.0354(10) Uani 1 1 d . . .
H10A H 0.835(6) 0.981(5) 0.059(4) 0.036(13) Uiso 1 1 d . . .
H10B H 0.950(7) 0.912(7) 0.070(6) 0.049(17) Uiso 1 1 d . . .
C11 C 1.0381(6) 1.0744(6) 0.2272(6) 0.0492(13) Uani 1 1 d . . .
H11B H 1.117(7) 1.028(7) 0.259(6) 0.062(17) Uiso 1 1 d . . .
H11A H 1.104(8) 1.147(7) 0.208(5) 0.054(17) Uiso 1 1 d . . .
C12 C 0.9613(8) 1.1271(6) 0.3146(6) 0.0561(15) Uani 1 1 d . . .
H12A H 0.916(8) 1.171(8) 0.277(6) 0.07(2) Uiso 1 1 d . . .
H12B H 1.054(8) 1.200(7) 0.403(6) 0.067(18) Uiso 1 1 d . . .
C13 C 0.7913(8) 1.0324(6) 0.4485(5) 0.0519(14) Uani 1 1 d . . .
H13A H 0.7967 1.1273 0.4685 0.062 Uiso 1 1 calc R A 1
H13B H 0.8727 1.0342 0.5174 0.062 Uiso 1 1 calc R A 1
C14A C 0.6139(10) 0.9174(8) 0.4294(6) 0.0510(18) Uani 0.804(11) 1 d P B 1
H14A H 0.5936 0.9279 0.5079 0.061 Uiso 0.804(11) 1 calc PR B 1
H14B H 0.5307 0.9313 0.3749 0.061 Uiso 0.804(11) 1 calc PR B 1
C14B C 0.700(4) 0.902(3) 0.474(3) 0.0510(18) Uani 0.196(11) 1 d P B 2
H14C H 0.6322 0.9209 0.5232 0.061 Uiso 0.196(11) 1 calc PR B 2
H14D H 0.7845 0.8877 0.5260 0.061 Uiso 0.196(11) 1 calc PR B 2
C15 C 0.5867(7) 0.7677(6) 0.3759(5) 0.0438(11) Uani 1 1 d . . .
H15A H 0.468(7) 0.700(7) 0.344(5) 0.053(16) Uiso 1 1 d . . .
H15B H 0.657(7) 0.736(7) 0.434(6) 0.066(18) Uiso 1 1 d . . .
C16 C 0.5667(7) 0.3854(8) 0.3444(5) 0.0546(15) Uani 1 1 d . . .
H16A H 0.446(7) 0.375(6) 0.348(5) 0.054(15) Uiso 1 1 d . . .
H16B H 0.600(11) 0.437(10) 0.297(8) 0.12(3) 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C1 W1 N2 91.08(14) . 2_665 y
C1 W1 N1 92.86(14) . . y
N2 W1 N1 172.36(12) 2_665 . y
C1 W1 N4 94.31(15) . . y
N2 W1 N4 93.17(13) 2_665 . y
N1 W1 N4 93.05(13) . . y
C1 W1 N5 155.50(15) . . y
N2 W1 N5 90.70(13) 2_665 . y
N1 W1 N5 88.42(12) . . y
N4 W1 N5 61.20(13) . . y
C1 W1 C1 109.34(11) . 2_665 y
N2 W1 C1 86.77(13) 2_665 2_665 y
N1 W1 C1 85.76(12) . 2_665 y
N4 W1 C1 156.35(14) . 2_665 y
N5 W1 C1 95.16(13) . 2_665 y
C1 W1 W1 61.31(11) . 2_665 y
N2 W1 W1 87.85(9) 2_665 2_665 y
N1 W1 W1 88.31(9) . 2_665 y
N4 W1 W1 155.62(10) . 2_665 y
N5 W1 W1 143.18(9) . 2_665 y
C1 W1 W1 48.03(9) 2_665 2_665 y
C1 W1 C9 124.89(14) . . y
N2 W1 C9 90.36(12) 2_665 . y
N1 W1 C9 92.74(12) . . y
N4 W1 C9 30.65(13) . . y
N5 W1 C9 30.66(13) . . y
C1 W1 C9 125.74(13) 2_665 . y
W1 W1 C9 173.60(9) 2_665 . y
C2 N1 C3 117.8(3) . . y
C2 N1 W1 121.2(2) . . y
C3 N1 W1 120.6(3) . . y
C2 N2 C8 113.8(3) . . y
C2 N2 W1 121.3(3) . 2_665 y
C8 N2 W1 124.9(2) . 2_665 y
C2 N3 C5 121.0(4) . . y
C2 N3 C6 121.0(4) . . y
C5 N3 C6 111.6(3) . . y
C9 N4 C15 120.1(4) . . y
C9 N4 W1 93.9(3) . . y
C15 N4 W1 145.1(3) . . y
C9 N5 C10 120.8(4) . . y
C9 N5 W1 92.7(2) . . y
C10 N5 W1 145.3(3) . . y
C9 N6 C13 119.9(4) . . y
C9 N6 C12 119.8(4) . . y
C13 N6 C12 119.9(4) . . y
O1 C1 W1 167.0(3) . . y
O1 C1 W1 122.4(3) . 2_665 y
W1 C1 W1 70.66(11) . 2_665 y
N1 C2 N2 119.5(3) . . y
N1 C2 N3 123.0(3) . . y
N2 C2 N3 117.5(4) . . y
N1 C3 C4 112.8(4) . . n
C5 C4 C3 108.8(4) . . n
N3 C5 C4 110.5(4) . . n
N3 C6 C7 113.3(4) . . n
C8 C7 C6 107.8(4) . . n
N2 C8 C7 109.9(3) . . n
N5 C9 N4 111.8(4) . . y
N5 C9 N6 124.0(4) . . y
N4 C9 N6 124.3(4) . . y
N5 C9 W1 56.6(2) . . n
N4 C9 W1 55.4(2) . . n
N6 C9 W1 175.5(3) . . n
N5 C10 C11 110.0(4) . . n
C12 C11 C10 111.0(4) . . n
N6 C12 C11 110.3(5) . . n
C14B C13 N6 112.9(11) . . n
N6 C13 C14A 111.2(5) . . n
C15 C14A C13 112.3(5) . . n
C13 C14B C15 120(2) . . n
C14B C15 N4 114.2(12) . . n
N4 C15 C14A 111.0(4) . . n
Cl2 C16 Cl1 111.6(3) . . n
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
W1 C1 1.944(4) . y
W1 N2 2.128(3) 2_665 y
W1 N1 2.138(3) . y
W1 N4 2.153(4) . y
W1 N5 2.181(3) . y
W1 C1 2.294(4) 2_665 y
W1 W1 2.4675(3) 2_665 y
W1 C9 2.609(4) . y
Cl1 C16 1.761(6) . n
Cl2 C16 1.750(7) . n
O1 C1 1.188(5) . y
N1 C2 1.349(5) . y
N1 C3 1.478(5) . y
N2 C2 1.357(5) . y
N2 C8 1.463(5) . y
N2 W1 2.128(3) 2_665 y
N3 C2 1.385(5) . y
N3 C5 1.463(6) . y
N3 C6 1.464(6) . y
N4 C9 1.333(6) . y
N4 C15 1.449(6) . y
N5 C9 1.332(5) . y
N5 C10 1.449(5) . y
N6 C9 1.360(6) . y
N6 C13 1.453(7) . y
N6 C12 1.464(7) . y
C1 W1 2.294(4) 2_665 y
C3 C4 1.511(6) . n
C4 C5 1.499(7) . n
C6 C7 1.521(6) . n
C7 C8 1.517(6) . n
C10 C11 1.521(7) . n
C11 C12 1.509(9) . n
C13 C14B 1.44(3) . n
C13 C14A 1.504(10) . n
C14A C15 1.498(9) . n
C14B C15 1.44(3) . n
