#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:09:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179829 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/25/7012546.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_7012546
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         'C17 H16 O3 W'
_chemical_formula_sum            'C17 H16 O3 W'
_chemical_formula_weight         452.15
_chemical_name_common
;(1,2,3,4,5-pentamethyl
cyclopentadienyl)(tricarbonyl)tungsten(buta-1,3-diynyl)
;
_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                   19.1104(5)
_cell_length_b                   10.8040(3)
_cell_length_c                   7.4292(2)
_cell_measurement_reflns_used    7101
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.463
_cell_measurement_theta_min      2.166
_cell_volume                     1533.90(7)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16022
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    7.537
_exptl_absorpt_correction_T_max  0.323
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G.M.Sheldrick, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.978
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0227
_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)+(0.0110P)²+3.9836P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0446
_reflns_number_gt                1587
_reflns_number_total             1853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212074g.txt
_cod_data_source_block           01srv144Compound1
_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      Pnma
_cod_database_code               7012546
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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.402011(10) 0.2500 0.75942(2) 0.01522(6) Uani 1 2 d S . .
O21 O 0.42472(15) -0.0019(3) 0.5536(4) 0.0325(7) Uani 1 1 d . . .
O22 O 0.5668(2) 0.2500 0.7217(6) 0.0318(9) Uani 1 2 d S . .
C1 C 0.3246(3) 0.2500 0.5507(7) 0.0217(11) Uani 1 2 d S . .
C2 C 0.2783(3) 0.2500 0.4480(7) 0.0197(11) Uani 1 2 d S . .
C3 C 0.2186(3) 0.2500 0.3336(7) 0.0238(12) Uani 1 2 d S . .
C4 C 0.1673(3) 0.2500 0.2377(9) 0.0290(12) Uani 1 2 d S . .
H4 H 0.123(3) 0.2500 0.154(9) 0.035 Uiso 1 2 d S . .
C01 C 0.4146(3) 0.2500 1.0772(7) 0.0182(10) Uani 1 2 d S . .
C02 C 0.37497(19) 0.1424(3) 1.0264(5) 0.0166(7) Uani 1 1 d . . .
C03 C 0.31121(18) 0.1827(3) 0.9443(5) 0.0166(7) Uani 1 1 d . . .
C11 C 0.4818(3) 0.2500 1.1793(8) 0.0225(12) Uani 1 2 d S . .
H11A H 0.468(3) 0.2500 1.303(8) 0.022(15) Uiso 1 2 d S . .
H11B H 0.510(2) 0.182(4) 1.155(6) 0.032(12) Uiso 1 1 d . . .
C12 C 0.3930(2) 0.0117(4) 1.0746(5) 0.0217(8) Uani 1 1 d . . .
H12A H 0.379(2) -0.007(4) 1.183(6) 0.033 Uiso 1 1 d . . .
H12B H 0.444(2) 0.002(4) 1.086(6) 0.033 Uiso 1 1 d . . .
H12C H 0.372(2) -0.044(4) 0.991(6) 0.033 Uiso 1 1 d . . .
C13 C 0.2519(2) 0.1013(4) 0.8859(6) 0.0234(8) Uani 1 1 d . . .
H13A H 0.264(2) 0.029(4) 0.840(6) 0.035 Uiso 1 1 d . . .
H13B H 0.220(2) 0.143(4) 0.808(6) 0.035 Uiso 1 1 d . . .
H13C H 0.223(2) 0.085(4) 0.980(6) 0.035 Uiso 1 1 d . . .
C21 C 0.41845(19) 0.0916(4) 0.6234(5) 0.0206(8) Uani 1 1 d . . .
C22 C 0.5075(2) 0.2500 0.7385(7) 0.0154(9) Uani 1 2 d S . .
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
C21 W1 C21 116.5(2) . 7_565 yes
C21 W1 C22 78.79(12) . . yes
C21 W1 C22 78.79(12) 7_565 . ?
C21 W1 C1 75.20(12) . . yes
C21 W1 C1 75.20(12) 7_565 . yes
C22 W1 C1 129.3(2) . . ?
C21 W1 C03 132.67(13) . 7_565 ?
C21 W1 C03 98.46(13) 7_565 7_565 ?
C22 W1 C03 142.02(15) . 7_565 ?
C1 W1 C03 84.95(16) . 7_565 ?
C21 W1 C03 98.46(13) . . ?
C21 W1 C03 132.67(13) 7_565 . ?
C22 W1 C03 142.02(15) . . ?
C1 W1 C03 84.95(16) . . ?
C03 W1 C03 36.36(17) 7_565 . ?
C21 W1 C02 151.24(14) . 7_565 ?
C21 W1 C02 92.14(13) 7_565 7_565 ?
C22 W1 C02 106.46(15) . 7_565 ?
C1 W1 C02 117.22(15) . 7_565 ?
C03 W1 C02 35.56(12) 7_565 7_565 ?
C03 W1 C02 59.62(12) . 7_565 ?
C21 W1 C02 92.14(13) . . ?
C21 W1 C02 151.24(14) 7_565 . ?
C22 W1 C02 106.46(15) . . ?
C1 W1 C02 117.22(15) . . ?
C03 W1 C02 59.62(12) 7_565 . ?
C03 W1 C02 35.56(12) . . ?
C02 W1 C02 59.13(17) 7_565 . ?
C21 W1 C01 118.94(11) . . ?
C21 W1 C01 118.94(11) 7_565 . ?
C22 W1 C01 88.61(19) . . ?
C1 W1 C01 142.13(19) . . ?
C03 W1 C01 59.25(14) 7_565 . ?
C03 W1 C01 59.25(14) . . ?
C02 W1 C01 35.39(11) 7_565 . ?
C02 W1 C01 35.39(11) . . ?
C2 C1 W1 174.5(5) . . yes
C1 C2 C3 175.9(6) . . yes
C4 C3 C2 179.4(6) . . yes
C02 C01 C02 108.0(4) . 7_565 ?
C02 C01 C11 125.9(2) . . ?
C02 C01 C11 125.9(2) 7_565 . ?
C02 C01 W1 71.7(2) . . ?
C02 C01 W1 71.7(2) 7_565 . ?
C11 C01 W1 126.4(4) . . ?
C03 C02 C01 108.3(3) . . ?
C03 C02 C12 125.9(3) . . ?
C01 C02 C12 125.4(3) . . ?
C03 C02 W1 71.17(19) . . ?
C01 C02 W1 72.9(2) . . ?
C12 C02 W1 128.0(2) . . ?
C02 C03 C03 107.7(2) . 7_565 ?
C02 C03 C13 126.0(3) . . ?
C03 C03 C13 125.9(2) 7_565 . ?
C02 C03 W1 73.27(19) . . ?
C03 C03 W1 71.82(8) 7_565 . ?
C13 C03 W1 125.2(2) . . ?
O21 C21 W1 175.5(3) . . ?
O22 C22 W1 178.1(5) . . ?
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 C21 2.012(4) . ?
W1 C21 2.012(4) 7_565 ?
W1 C22 2.023(5) . ?
W1 C1 2.143(6) . yes
W1 C03 2.329(3) 7_565 ?
W1 C03 2.329(3) . ?
W1 C02 2.357(3) 7_565 ?
W1 C02 2.357(3) . ?
W1 C01 2.373(5) . ?
O21 C21 1.141(5) . ?
O22 C22 1.140(6) . ?
C1 C2 1.169(8) . yes
C2 C3 1.422(8) . yes
C3 C4 1.212(8) . yes
C01 C02 1.438(5) . ?
C01 C02 1.438(5) 7_565 ?
C01 C11 1.492(7) . ?
C02 C03 1.431(5) . ?
C02 C12 1.496(5) . ?
C03 C03 1.453(7) 7_565 ?
C03 C13 1.500(5) . ?
