#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:09:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179829 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/25/7012548.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_7012548
loop_
_publ_author_name
'Roberts, Rachel L.'
'Puschmann, Horst'
'Howard, Judith A. K.'
'Yamamoto, John H.'
'Carty, Arthur J.'
'Low, Paul J.'
_publ_section_title
;
 Synthesis and structure of a series of tungsten(ii) and tungsten(vi)
 diynyl and diyndiyl complexes
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1099
_journal_paper_doi               10.1039/b212074g
_journal_year                    2003
_chemical_formula_moiety         'C14 H16 O3 W'
_chemical_formula_sum            'C14 H16 O3 W'
_chemical_formula_weight         416.12
_chemical_name_common
;(1,2,3,4,5-pentamethyl cyclopentadienyl)(oxo-
peroxo)tungsten(buta-1,3-diynyl)
;
_chemical_name_systematic
; 
? 
;
_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                 98.2000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7790(3)
_cell_length_b                   13.8399(5)
_cell_length_c                   12.7350(5)
_cell_measurement_reflns_used    5031
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.477
_cell_measurement_theta_min      3.027
_cell_volume                     1357.04(9)
_computing_cell_refinement       'SMART version 5.060 (Bruker, 1999)'
_computing_data_collection       'SMART version 5.060 (Bruker, 1999)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 5.10 (Bruker, 1997)'
_computing_publication_material  'SHELXTL version 5.10 (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15600
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    8.509
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G.M.Sheldrick, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.500
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0148P)²+3.9895P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0506
_reflns_number_gt                3112
_reflns_number_total             3424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212074g.txt
_cod_data_source_block           01srv159Compound3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012548
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.867293(18) 0.207952(10) 0.629470(11) 0.01432(5) Uani 1 1 d . . .
O1 O 0.8639(4) 0.3009(2) 0.7193(2) 0.0264(6) Uani 1 1 d . . .
O2 O 1.0642(5) 0.2250(2) 0.5548(3) 0.0366(8) Uani 1 1 d . . .
O3 O 0.9067(5) 0.2705(3) 0.4996(3) 0.0361(8) Uani 1 1 d . . .
C1 C 1.0396(5) 0.1158(3) 0.7228(3) 0.0193(7) Uani 1 1 d . . .
C2 C 1.1365(5) 0.0640(3) 0.7812(3) 0.0188(7) Uani 1 1 d . . .
C3 C 1.2404(5) 0.0027(3) 0.8492(3) 0.0209(8) Uani 1 1 d . . .
C4 C 1.3295(6) -0.0507(3) 0.9061(4) 0.0269(9) Uani 1 1 d . . .
H4 H 1.386(7) -0.085(4) 0.938(4) 0.033(15) Uiso 1 1 d . . .
C01 C 0.5727(5) 0.1809(3) 0.6624(3) 0.0172(7) Uani 1 1 d . . .
C02 C 0.6659(5) 0.0949(3) 0.6900(3) 0.0160(7) Uani 1 1 d . . .
C03 C 0.7157(5) 0.0533(3) 0.5934(3) 0.0156(7) Uani 1 1 d . . .
C04 C 0.6583(5) 0.1156(3) 0.5083(3) 0.0161(7) Uani 1 1 d . . .
C05 C 0.5772(5) 0.1980(3) 0.5516(3) 0.0164(7) Uani 1 1 d . . .
C11 C 0.4886(5) 0.2452(3) 0.7346(3) 0.0241(9) Uani 1 1 d . . .
H11A H 0.3701 0.2226 0.7379 0.036 Uiso 1 1 calc R . .
H11B H 0.4848 0.3115 0.7073 0.036 Uiso 1 1 calc R . .
H11C H 0.5557 0.2436 0.8058 0.036 Uiso 1 1 calc R . .
C12 C 0.6908(5) 0.0470(3) 0.7967(3) 0.0246(8) Uani 1 1 d . . .
H12A H 0.5919 0.0045 0.8026 0.037 Uiso 1 1 calc R . .
H12B H 0.6987 0.0965 0.8523 0.037 Uiso 1 1 calc R . .
H12C H 0.7980 0.0089 0.8050 0.037 Uiso 1 1 calc R . .
C13 C 0.7999(5) -0.0434(3) 0.5860(4) 0.0248(8) Uani 1 1 d . . .
H13A H 0.7101 -0.0931 0.5711 0.037 Uiso 1 1 calc R . .
H13B H 0.8730 -0.0580 0.6534 0.037 Uiso 1 1 calc R . .
H13C H 0.8718 -0.0423 0.5288 0.037 Uiso 1 1 calc R . .
C14 C 0.6804(5) 0.1024(3) 0.3945(3) 0.0228(8) Uani 1 1 d . . .
H14A H 0.5841 0.0636 0.3586 0.034 Uiso 1 1 calc R . .
H14B H 0.7905 0.0692 0.3902 0.034 Uiso 1 1 calc R . .
H14C H 0.6810 0.1657 0.3601 0.034 Uiso 1 1 calc R . .
C15 C 0.4925(6) 0.2809(3) 0.4879(3) 0.0256(8) Uani 1 1 d . . .
H15A H 0.3716 0.2644 0.4613 0.038 Uiso 1 1 calc R . .
H15B H 0.5551 0.2940 0.4278 0.038 Uiso 1 1 calc R . .
H15C H 0.4954 0.3385 0.5329 0.038 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 0.0000 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'
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
O1 W1 O2 108.92(15) . . yes
O1 W1 O3 104.66(15) . . yes
O2 W1 O3 44.64(15) . . yes
O1 W1 C1 98.48(14) . . yes
O2 W1 C1 82.25(15) . . ?
O3 W1 C1 126.37(15) . . ?
O1 W1 C05 102.73(13) . . ?
O2 W1 C05 125.79(14) . . ?
O3 W1 C05 85.66(14) . . ?
C1 W1 C05 134.97(14) . . ?
O1 W1 C01 84.03(13) . . ?
O2 W1 C01 160.67(14) . . ?
O3 W1 C01 119.25(14) . . ?
C1 W1 C01 110.68(14) . . ?
C05 W1 C01 35.13(12) . . ?
O1 W1 C02 101.54(13) . . ?
O2 W1 C02 146.35(13) . . ?
O3 W1 C02 138.86(13) . . ?
C1 W1 C02 79.39(14) . . ?
C05 W1 C02 57.75(13) . . ?
C01 W1 C02 33.97(12) . . ?
O1 W1 C04 137.68(13) . . ?
O2 W1 C04 104.87(14) . . ?
O3 W1 C04 82.28(13) . . ?
C1 W1 C04 110.79(14) . . ?
C05 W1 C04 35.29(12) . . ?
C01 W1 C04 57.69(12) . . ?
C02 W1 C04 57.20(12) . . ?
O1 W1 C03 136.24(13) . . ?
O2 W1 C03 114.09(13) . . ?
O3 W1 C03 111.19(13) . . ?
C1 W1 C03 80.01(13) . . ?
C05 W1 C03 57.32(12) . . ?
C01 W1 C03 57.00(12) . . ?
C02 W1 C03 34.84(12) . . ?
C04 W1 C03 33.42(12) . . ?
O3 O2 W1 67.69(18) . . yes
O2 O3 W1 67.68(18) . . yes
C2 C1 W1 176.9(3) . . yes
C1 C2 C3 177.3(4) . . yes
C4 C3 C2 178.9(5) . . yes
C02 C01 C05 107.4(3) . . ?
C02 C01 C11 127.1(4) . . ?
C05 C01 C11 125.4(4) . . ?
C02 C01 W1 73.0(2) . . ?
C05 C01 W1 69.4(2) . . ?
C11 C01 W1 121.6(3) . . ?
C01 C02 C03 108.2(3) . . ?
C01 C02 C12 126.4(3) . . ?
C03 C02 C12 125.1(3) . . ?
C01 C02 W1 73.0(2) . . ?
C03 C02 W1 74.0(2) . . ?
C12 C02 W1 124.7(3) . . ?
C04 C03 C02 108.3(3) . . ?
C04 C03 C13 126.3(3) . . ?
C02 C03 C13 125.2(3) . . ?
C04 C03 W1 72.6(2) . . ?
C02 C03 W1 71.13(19) . . ?
C13 C03 W1 126.0(2) . . ?
C03 C04 C05 107.3(3) . . ?
C03 C04 C14 127.2(3) . . ?
C05 C04 C14 125.5(3) . . ?
C03 C04 W1 74.0(2) . . ?
C05 C04 W1 68.5(2) . . ?
C14 C04 W1 121.3(2) . . ?
C01 C05 C04 108.5(3) . . ?
C01 C05 C15 125.9(3) . . ?
C04 C05 C15 125.2(3) . . ?
C01 C05 W1 75.5(2) . . ?
C04 C05 W1 76.2(2) . . ?
C15 C05 W1 120.5(3) . . ?
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 O1 1.724(3) . yes
W1 O2 1.929(3) . yes
W1 O3 1.929(3) . yes
W1 C1 2.093(4) . yes
W1 C05 2.336(4) . ?
W1 C01 2.417(4) . ?
W1 C02 2.417(3) . ?
W1 C04 2.438(4) . ?
W1 C03 2.456(4) . ?
O2 O3 1.465(5) . yes
C1 C2 1.215(5) . yes
C2 C3 1.387(6) . yes
C3 C4 1.187(6) . yes
C01 C02 1.412(5) . ?
C01 C05 1.436(5) . ?
C01 C11 1.495(5) . ?
C02 C03 1.459(5) . ?
C02 C12 1.499(5) . ?
C03 C04 1.407(5) . ?
C03 C13 1.499(5) . ?
C04 C05 1.450(5) . ?
C04 C14 1.495(5) . ?
C05 C15 1.502(5) . ?
