#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:09:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179829 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/25/7012549.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_7012549
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 O2 W'
_chemical_formula_sum            'C14 H16 O2 W'
_chemical_formula_weight         400.12
_chemical_name_common
;(1,2,3,4,5-pentamethyl cyclopentadienyl)(dioxo)tungsten(buta-
1,3-diynyl)
;
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   12.5473(11)
_cell_length_b                   12.6869(11)
_cell_length_c                   17.0809(16)
_cell_measurement_reflns_used    6073
_cell_measurement_temperature    393(2)
_cell_measurement_theta_max      34.815
_cell_measurement_theta_min      2.576
_cell_volume                     2719.0(4)
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL version 6.12 (Bruker, 2001)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD 6K 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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28375
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    8.484
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.6701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G.M.Sheldrick, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.686
_refine_diff_density_min         -1.841
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0212
_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)+(0.0000P)²+6.6022P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                2563
_reflns_number_total             2964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212074g.txt
_cod_data_source_block           02srv059Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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      Pbca
_cod_database_code               7012549
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.145827(11) 0.170157(12) 0.620554(8) 0.02198(7) Uani 1 1 d . . .
O1 O 0.1173(3) 0.0457(2) 0.65713(18) 0.0390(7) Uani 1 1 d . . .
O2 O 0.2573(2) 0.2170(3) 0.66823(18) 0.0426(8) Uani 1 1 d . . .
C1 C 0.2046(3) 0.1397(3) 0.5088(2) 0.0251(8) Uani 1 1 d . . .
C2 C 0.2434(3) 0.1171(3) 0.4467(2) 0.0241(7) Uani 1 1 d . . .
C3 C 0.2870(3) 0.0877(3) 0.3759(2) 0.0246(8) Uani 1 1 d . . .
C4 C 0.3224(3) 0.0574(3) 0.3147(3) 0.0316(9) Uani 1 1 d . . .
H4 H 0.344(5) 0.032(5) 0.267(4) 0.065(19) Uiso 1 1 d . . .
C01 C -0.0431(3) 0.2026(3) 0.6297(2) 0.0222(7) Uani 1 1 d . . .
C02 C -0.0202(3) 0.2209(3) 0.5509(2) 0.0216(7) Uani 1 1 d . . .
C03 C 0.0512(3) 0.3101(3) 0.5465(2) 0.0225(7) Uani 1 1 d . . .
C04 C 0.0717(3) 0.3463(3) 0.6231(2) 0.0227(8) Uani 1 1 d . . .
C05 C 0.0184(3) 0.2753(3) 0.6761(2) 0.0214(7) Uani 1 1 d . . .
C11 C -0.1174(4) 0.1204(4) 0.6618(3) 0.0381(10) Uani 1 1 d . . .
H11A H -0.1795 0.1157 0.6291 0.057 Uiso 1 1 calc R . .
H11B H -0.1384 0.1395 0.7139 0.057 Uiso 1 1 calc R . .
H11C H -0.0819 0.0534 0.6628 0.057 Uiso 1 1 calc R . .
C12 C -0.0638(4) 0.1631(3) 0.4813(2) 0.0328(9) Uani 1 1 d . . .
H12A H -0.0963 0.0985 0.4982 0.049 Uiso 1 1 calc R . .
H12B H -0.0070 0.1476 0.4455 0.049 Uiso 1 1 calc R . .
H12C H -0.1161 0.2062 0.4556 0.049 Uiso 1 1 calc R . .
C13 C 0.0880(4) 0.3613(4) 0.4721(2) 0.0351(9) Uani 1 1 d . . .
H13A H 0.0333 0.4075 0.4529 0.053 Uiso 1 1 calc R . .
H13B H 0.1027 0.3080 0.4337 0.053 Uiso 1 1 calc R . .
H13C H 0.1515 0.4012 0.4821 0.053 Uiso 1 1 calc R . .
C14 C 0.1396(4) 0.4373(4) 0.6469(3) 0.0430(11) Uani 1 1 d . . .
H14A H 0.1817 0.4181 0.6916 0.064 Uiso 1 1 calc R . .
H14B H 0.0950 0.4962 0.6600 0.064 Uiso 1 1 calc R . .
H14C H 0.1858 0.4563 0.6044 0.064 Uiso 1 1 calc R . .
C15 C 0.0165(4) 0.2836(4) 0.7643(2) 0.0338(9) Uani 1 1 d . . .
H15A H 0.0801 0.3180 0.7820 0.051 Uiso 1 1 calc R . .
H15B H 0.0127 0.2142 0.7866 0.051 Uiso 1 1 calc R . .
H15C H -0.0447 0.3237 0.7803 0.051 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
O2 W1 O1 108.09(17) . . yes
O2 W1 C1 102.12(15) . . ?
O1 W1 C1 103.53(15) . . yes
O2 W1 C05 99.78(14) . . ?
O1 W1 C05 103.72(14) . . ?
C1 W1 C05 137.37(14) . . ?
O2 W1 C01 135.11(14) . . ?
O1 W1 C01 85.94(14) . . ?
C1 W1 C01 116.03(13) . . ?
C05 W1 C01 35.61(13) . . ?
O2 W1 C04 89.15(15) . . ?
O1 W1 C04 138.94(14) . . ?
C1 W1 C04 108.92(14) . . ?
C05 W1 C04 35.48(13) . . ?
C01 W1 C04 57.56(13) . . ?
O2 W1 C03 112.47(15) . . ?
O1 W1 C03 137.36(14) . . ?
C1 W1 C03 80.53(13) . . ?
C05 W1 C03 57.30(12) . . ?
C01 W1 C03 55.98(12) . . ?
C04 W1 C03 33.39(12) . . ?
O2 W1 C02 144.84(15) . . ?
O1 W1 C02 103.61(14) . . ?
C1 W1 C02 84.59(13) . . ?
C05 W1 C02 57.44(12) . . ?
C01 W1 C02 33.09(12) . . ?
C04 W1 C02 56.45(12) . . ?
C03 W1 C02 33.85(12) . . ?
C2 C1 W1 175.4(3) . . yes
C1 C2 C3 178.0(4) . . yes
C4 C3 C2 176.8(4) . . yes
C02 C01 C05 108.3(3) . . ?
C02 C01 C11 126.5(4) . . ?
C05 C01 C11 125.2(4) . . ?
C02 C01 W1 76.3(2) . . ?
C05 C01 W1 67.55(19) . . ?
C11 C01 W1 121.0(3) . . ?
C01 C02 C03 107.9(3) . . ?
C01 C02 C12 127.4(4) . . ?
C03 C02 C12 124.6(3) . . ?
C01 C02 W1 70.6(2) . . ?
C03 C02 W1 73.0(2) . . ?
C12 C02 W1 124.0(3) . . ?
C04 C03 C02 108.7(3) . . ?
C04 C03 C13 126.1(4) . . ?
C02 C03 C13 125.0(3) . . ?
C04 C03 W1 70.9(2) . . ?
C02 C03 W1 73.1(2) . . ?
C13 C03 W1 126.4(3) . . ?
C03 C04 C05 107.2(3) . . ?
C03 C04 C14 127.5(4) . . ?
C05 C04 C14 125.3(4) . . ?
C03 C04 W1 75.7(2) . . ?
C05 C04 W1 67.2(2) . . ?
C14 C04 W1 120.0(3) . . ?
C04 C05 C01 107.6(3) . . ?
C04 C05 C15 126.2(3) . . ?
C01 C05 C15 125.8(3) . . ?
C04 C05 W1 77.3(2) . . ?
C01 C05 W1 76.8(2) . . ?
C15 C05 W1 117.7(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 O2 1.724(3) . yes
W1 O1 1.735(3) . yes
W1 C1 2.082(4) . yes
W1 C05 2.288(4) . ?
W1 C01 2.411(4) . ?
W1 C04 2.421(4) . ?
W1 C03 2.483(4) . ?
W1 C02 2.484(3) . ?
C1 C2 1.202(5) . yes
C2 C3 1.379(5) . yes
C3 C4 1.200(6) . yes
C01 C02 1.396(5) . ?
C01 C05 1.442(5) . ?
C01 C11 1.503(6) . ?
C02 C03 1.446(5) . ?
C02 C12 1.500(5) . ?
C03 C04 1.410(5) . ?
C03 C13 1.500(5) . ?
C04 C05 1.441(5) . ?
C04 C14 1.492(6) . ?
C05 C15 1.510(5) . ?
