#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:43:06 +0100 (lun 21 de mar de 2016) $
#$Revision: 178664 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/75/4077526.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_4077526
loop_
_publ_author_name
'Johnson, Brian P.'
'Schiffer, Michael'
'Scheer, Manfred'
_publ_section_title
;
 Novel Approach to Intermediates Containing a Tungsten−Arsenic
 Triple Bond†
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3404
_journal_paper_doi               10.1021/om0003436
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C12 H15 As3 O2 W'
_chemical_formula_weight         599.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   8.5450(17)
_cell_length_b                   13.506(3)
_cell_length_c                   13.253(3)
_cell_measurement_reflns_used    1049
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.15
_cell_volume                     1529.5(6)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software'
_computing_molecular_graphics    SIEMENS-XP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9427
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    13.984
_exptl_absorpt_correction_T_max  0.3300
_exptl_absorpt_correction_T_min  0.2041
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'program faceit'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0269
_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)+(0.0385P)²+4.5205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                1417
_reflns_number_total             1541
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0003436.cif
_cod_data_source_block           fin
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        1529.5(5)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4077526
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
W W 0.07460(3) 0.7500 0.012822(19) 0.02207(12) Uani 1 2 d S
As1 As 0.08344(8) 0.66139(5) -0.16380(4) 0.04087(19) Uani 1 1 d .
As2 As -0.15109(11) 0.7500 -0.12994(6) 0.0450(2) Uani 1 2 d S
C1 C -0.0777(6) 0.6460(4) 0.0576(4) 0.0327(12) Uani 1 1 d .
O1 O -0.1574(6) 0.5863(4) 0.0870(4) 0.0530(12) Uani 1 1 d .
C2 C 0.1942(8) 0.7500 0.1676(5) 0.0266(14) Uani 1 2 d S
C3 C 0.2499(6) 0.6643(3) 0.1148(4) 0.0270(10) Uani 1 1 d .
C4 C 0.3374(6) 0.6967(4) 0.0300(4) 0.0274(10) Uani 1 1 d .
C5 C 0.1103(11) 0.7500 0.2681(6) 0.0392(18) Uani 1 2 d S
H5A H 0.1855 0.7400 0.3219 0.059 Uiso 0.50 1 calc PR
H5B H 0.0337 0.6970 0.2692 0.059 Uiso 0.50 1 calc PR
H5C H 0.0577 0.8130 0.2775 0.059 Uiso 0.50 1 calc PR
C6 C 0.2370(7) 0.5581(4) 0.1500(4) 0.0383(13) Uani 1 1 d .
H6A H 0.1479 0.5516 0.1949 0.057 Uiso 1 1 calc R
H6B H 0.3317 0.5396 0.1855 0.057 Uiso 1 1 calc R
H6C H 0.2229 0.5151 0.0921 0.057 Uiso 1 1 calc R
C7 C 0.4338(7) 0.6327(5) -0.0393(5) 0.0416(14) Uani 1 1 d .
H7A H 0.3820 0.5695 -0.0487 0.062 Uiso 1 1 calc R
H7B H 0.5363 0.6220 -0.0098 0.062 Uiso 1 1 calc R
H7C H 0.4453 0.6654 -0.1041 0.062 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W 0.02330(18) 0.02213(17) 0.02078(17) 0.000 -0.00191(10) 0.000
As1 0.0564(4) 0.0372(3) 0.0290(3) -0.0078(2) -0.0010(2) 0.0025(3)
As2 0.0373(5) 0.0650(6) 0.0326(4) 0.000 -0.0103(4) 0.000
C1 0.031(3) 0.038(3) 0.029(3) -0.001(2) -0.004(2) 0.002(2)
O1 0.049(3) 0.049(2) 0.061(3) 0.007(2) -0.001(2) -0.020(2)
C2 0.024(3) 0.031(3) 0.024(3) 0.000 -0.002(3) 0.000
C3 0.025(3) 0.026(2) 0.030(2) 0.0022(19) -0.011(2) 0.0008(19)
C4 0.022(3) 0.031(3) 0.029(2) 0.000(2) -0.0042(19) 0.004(2)
C5 0.041(5) 0.046(4) 0.031(4) 0.000 0.000(3) 0.000
C6 0.047(3) 0.028(3) 0.041(3) 0.008(2) -0.005(2) 0.000(2)
C7 0.033(3) 0.044(3) 0.048(3) -0.007(3) 0.008(3) 0.003(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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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
C1 W C1 88.9(3) . 7_575
C1 W C2 91.4(2) . .
C1 W C2 91.4(2) 7_575 .
C1 W C3 84.11(19) . .
C1 W C3 126.5(2) 7_575 .
C2 W C3 36.16(15) . .
C1 W C3 126.5(2) . 7_575
C1 W C3 84.1(2) 7_575 7_575
C2 W C3 36.16(15) . 7_575
C3 W C3 59.7(2) . 7_575
C1 W C4 112.0(2) . .
C1 W C4 143.11(19) 7_575 .
C2 W C4 59.4(2) . .
C3 W C4 35.17(18) . .
C3 W C4 59.00(17) 7_575 .
C1 W C4 143.11(19) . 7_575
C1 W C4 112.0(2) 7_575 7_575
C2 W C4 59.4(2) . 7_575
C3 W C4 59.00(17) . 7_575
C3 W C4 35.17(18) 7_575 7_575
C4 W C4 35.4(3) . 7_575
C1 W As1 126.95(15) . 7_575
C1 W As1 87.92(16) 7_575 7_575
C2 W As1 141.61(12) . 7_575
C3 W As1 136.48(13) . 7_575
C3 W As1 105.80(12) 7_575 7_575
C4 W As1 101.33(12) . 7_575
C4 W As1 85.41(12) 7_575 7_575
C1 W As1 87.91(16) . .
C1 W As1 126.95(15) 7_575 .
C2 W As1 141.61(12) . .
C3 W As1 105.80(12) . .
C3 W As1 136.48(13) 7_575 .
C4 W As1 85.41(12) . .
C4 W As1 101.33(12) 7_575 .
As1 W As1 54.13(3) 7_575 .
C1 W As2 75.17(15) . .
C1 W As2 75.17(15) 7_575 .
C2 W As2 160.94(18) . .
C3 W As2 150.07(12) . .
C3 W As2 150.07(12) 7_575 .
C4 W As2 138.06(12) . .
C4 W As2 138.07(12) 7_575 .
As1 W As2 52.93(2) 7_575 .
As1 W As2 52.93(2) . .
As2 As1 As1 59.77(2) . 7_575
As2 As1 W 65.08(3) . .
As1 As1 W 62.932(16) 7_575 .
As1 As2 As1 60.46(4) 7_575 .
As1 As2 W 61.99(3) 7_575 .
As1 As2 W 61.99(3) . .
O1 C1 W 176.1(5) . .
C3 C2 C3 107.6(6) 7_575 .
C3 C2 C5 126.0(3) 7_575 .
C3 C2 C5 126.0(3) . .
C3 C2 W 73.2(3) 7_575 .
C3 C2 W 73.2(3) . .
C5 C2 W 125.2(5) . .
C4 C3 C2 108.2(4) . .
C4 C3 C6 125.1(5) . .
C2 C3 C6 126.2(5) . .
C4 C3 W 74.1(3) . .
C2 C3 W 70.6(3) . .
C6 C3 W 127.2(4) . .
C3 C4 C4 108.0(3) . 7_575
C3 C4 C7 126.5(5) . .
C4 C4 C7 125.0(3) 7_575 .
C3 C4 W 70.8(3) . .
C4 C4 W 72.32(13) 7_575 .
C7 C4 W 129.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W C1 2.004(6) .
W C1 2.004(6) 7_575
W C2 2.292(7) .
W C3 2.326(5) .
W C3 2.326(5) 7_575
W C4 2.369(5) .
W C4 2.369(5) 7_575
W As1 2.6301(7) 7_575
W As1 2.6301(7) .
W As2 2.7017(10) .
As1 As2 2.3770(11) .
As1 As1 2.3936(13) 7_575
As2 As1 2.3770(11) 7_575
C1 O1 1.126(7) .
C2 C3 1.434(6) 7_575
C2 C3 1.434(6) .
C2 C5 1.512(10) .
C3 C4 1.419(7) .
C3 C6 1.512(7) .
C4 C4 1.439(10) 7_575
C4 C7 1.507(8) .
