#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:04:17 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180221 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/07/7110734.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7110734
loop_
_publ_author_name
'Bartlett, Ian M.'
'Carlton, Susannah'
'Connelly, Neil G.'
'Harding, David J.'
'Hayward, Owen D.'
'Guy Orpen, A.'
'Ray, Christopher D.'
'Rieger, Philip H.'
_publ_section_title
;
 Structure and bonding in the d4/d3 alkyne redox pairs
 [WX(CO)(MeCCMe)Tp′]z (X = F, Cl, Br and I; z = 0 and 1):
 halide stabilisation of electron deficient metal alkyne complexes
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2403
_journal_paper_doi               10.1039/a907912b
_journal_year                    1999
_chemical_formula_sum            'C20 H28 B2 Cl F4 N6 O W'
_chemical_formula_weight         685.40
_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                87.723(7)
_cell_angle_beta                 84.451(12)
_cell_angle_gamma                85.235(12)
_cell_formula_units_Z            2
_cell_length_a                   8.1371(10)
_cell_length_b                   11.770(3)
_cell_length_c                   13.3634(15)
_cell_measurement_reflns_used    214
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      1.53
_cell_volume                     1268.8(4)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13128
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    4.712
_exptl_absorpt_correction_T_max  0.708635
_exptl_absorpt_correction_T_min  0.544219
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick 1996'
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0199
_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)+(0.0140P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0415
_reflns_number_gt                5066
_reflns_number_total             5733
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            907912bsup1.cif
_cod_data_source_block           '[WCl(CO)(MeCCMe)Tp'][BF4]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1268.8(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110734
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
W1 W -0.002933(15) -0.179620(10) -0.293953(9) 0.01527(4) Uani 1 1 d .
Cl1 Cl -0.12320(10) -0.12422(7) -0.44248(6) 0.02787(18) Uani 1 1 d .
O1 O 0.2604(3) 0.0051(2) -0.35087(17) 0.0373(6) Uani 1 1 d .
N1 N 0.1644(3) -0.3015(2) -0.38577(17) 0.0189(5) Uani 1 1 d .
N2 N 0.1631(3) -0.4162(2) -0.36037(17) 0.0182(5) Uani 1 1 d .
N3 N -0.1669(3) -0.3173(2) -0.27645(17) 0.0192(5) Uani 1 1 d .
N4 N -0.1042(3) -0.4269(2) -0.25591(17) 0.0182(5) Uani 1 1 d .
N5 N 0.1324(3) -0.2680(2) -0.18038(17) 0.0182(5) Uani 1 1 d .
N6 N 0.1495(3) -0.3860(2) -0.17607(17) 0.0187(5) Uani 1 1 d .
C1 C 0.1755(4) -0.0637(3) -0.3316(2) 0.0229(7) Uani 1 1 d .
C2 C -0.2731(4) -0.1467(3) -0.0910(2) 0.0329(8) Uani 1 1 d .
H2A H -0.2139 -0.1556 -0.0303 0.049 Uiso 1 1 calc R
H2B H -0.3180 -0.2189 -0.1038 0.049 Uiso 1 1 calc R
H2C H -0.3639 -0.0869 -0.0813 0.049 Uiso 1 1 calc R
C3 C -0.1576(4) -0.1146(3) -0.1776(2) 0.0222(7) Uani 1 1 d .
C4 C -0.0865(4) -0.0304(3) -0.2223(2) 0.0211(6) Uani 1 1 d .
C5 C -0.0763(4) 0.0950(3) -0.2226(3) 0.0318(8) Uani 1 1 d .
H5A H -0.0632 0.1249 -0.2921 0.048 Uiso 1 1 calc R
H5B H 0.0191 0.1120 -0.1878 0.048 Uiso 1 1 calc R
H5C H -0.1780 0.1308 -0.1879 0.048 Uiso 1 1 calc R
C6 C 0.2507(5) -0.6059(3) -0.4351(3) 0.0370(9) Uani 1 1 d .
H6A H 0.3225 -0.6337 -0.4936 0.055 Uiso 1 1 calc R
H6B H 0.1394 -0.6311 -0.4375 0.055 Uiso 1 1 calc R
H6C H 0.2962 -0.6364 -0.3733 0.055 Uiso 1 1 calc R
C7 C 0.2417(4) -0.4785(3) -0.4364(2) 0.0245(7) Uani 1 1 d .
C8 C 0.2996(4) -0.4025(3) -0.5102(2) 0.0292(8) Uani 1 1 d .
H8 H 0.3613 -0.4214 -0.5722 0.035 Uiso 1 1 calc R
C9 C 0.2514(4) -0.2939(3) -0.4776(2) 0.0234(7) Uani 1 1 d .
C10 C 0.2886(4) -0.1834(3) -0.5315(2) 0.0345(8) Uani 1 1 d .
H10A H 0.3360 -0.1984 -0.6004 0.052 Uiso 1 1 calc R
H10B H 0.3681 -0.1459 -0.4960 0.052 Uiso 1 1 calc R
H10C H 0.1861 -0.1336 -0.5332 0.052 Uiso 1 1 calc R
C11 C -0.1972(4) -0.6218(3) -0.2269(3) 0.0353(8) Uani 1 1 d .
H11A H -0.3033 -0.6561 -0.2151 0.053 Uiso 1 1 calc R
H11B H -0.1351 -0.6362 -0.1677 0.053 Uiso 1 1 calc R
H11C H -0.1329 -0.6556 -0.2857 0.053 Uiso 1 1 calc R
C12 C -0.2277(4) -0.4970(3) -0.2452(2) 0.0247(7) Uani 1 1 d .
C13 C -0.3737(4) -0.4312(3) -0.2576(2) 0.0267(7) Uani 1 1 d .
H13 H -0.4817 -0.4572 -0.2532 0.032 Uiso 1 1 calc R
C14 C -0.3325(4) -0.3198(3) -0.2776(2) 0.0226(7) Uani 1 1 d .
C15 C -0.4471(4) -0.2189(3) -0.3004(3) 0.0331(8) Uani 1 1 d .
H15A H -0.5612 -0.2352 -0.2779 0.050 Uiso 1 1 calc R
H15B H -0.4374 -0.2022 -0.3731 0.050 Uiso 1 1 calc R
H15C H -0.4181 -0.1529 -0.2653 0.050 Uiso 1 1 calc R
C16 C 0.2663(5) -0.5453(3) -0.0678(3) 0.0387(9) Uani 1 1 d .
H16A H 0.3164 -0.5520 -0.0038 0.058 Uiso 1 1 calc R
H16B H 0.3427 -0.5821 -0.1202 0.058 Uiso 1 1 calc R
H16C H 0.1624 -0.5826 -0.0607 0.058 Uiso 1 1 calc R
C17 C 0.2319(4) -0.4215(3) -0.0963(2) 0.0241(7) Uani 1 1 d .
C18 C 0.2688(4) -0.3265(3) -0.0482(2) 0.0256(7) Uani 1 1 d .
H18 H 0.3264 -0.3261 0.0103 0.031 Uiso 1 1 calc R
C19 C 0.2058(4) -0.2320(3) -0.1014(2) 0.0197(6) Uani 1 1 d .
C20 C 0.2138(4) -0.1100(3) -0.0789(2) 0.0293(8) Uani 1 1 d .
H20A H 0.2770 -0.1046 -0.0207 0.044 Uiso 1 1 calc R
H20B H 0.1014 -0.0744 -0.0638 0.044 Uiso 1 1 calc R
H20C H 0.2684 -0.0705 -0.1373 0.044 Uiso 1 1 calc R
B1 B 0.0828(4) -0.4544(3) -0.2575(3) 0.0193(7) Uani 1 1 d .
H1 H 0.107(3) -0.546(2) -0.2442(18) 0.009(7) Uiso 1 1 d .
B2 B 0.4404(5) 0.1699(3) -0.1825(3) 0.0270(8) Uani 1 1 d .
F1 F 0.5106(3) 0.06744(19) -0.21909(19) 0.0635(7) Uani 1 1 d .
F2 F 0.4592(3) 0.25457(19) -0.25652(15) 0.0491(6) Uani 1 1 d .
F3 F 0.2734(2) 0.16297(19) -0.15373(15) 0.0446(5) Uani 1 1 d .
F4 F 0.5206(2) 0.19808(19) -0.10113(14) 0.0433(5) Uani 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
C3 W1 C4 36.54(11)
C3 W1 C1 107.35(12)
C4 W1 C1 73.20(12)
C3 W1 N5 85.83(10)
C4 W1 N5 100.85(10)
C1 W1 N5 94.13(10)
C3 W1 N3 82.67(11)
C4 W1 N3 116.45(11)
C1 W1 N3 169.98(10)
N5 W1 N3 86.80(9)
C3 W1 N1 160.63(10)
C4 W1 N1 158.93(10)
C1 W1 N1 85.77(10)
N5 W1 N1 78.91(9)
N3 W1 N1 84.62(9)
C3 W1 Cl1 107.20(8)
C4 W1 Cl1 94.06(8)
C1 W1 Cl1 89.02(8)
N5 W1 Cl1 165.04(6)
N3 W1 Cl1 87.61(7)
N1 W1 Cl1 86.75(6)
C9 N1 N2 106.5(2)
C9 N1 W1 133.8(2)
N2 N1 W1 118.25(17)
C7 N2 N1 109.8(2)
C7 N2 B1 130.3(3)
N1 N2 B1 119.9(2)
C14 N3 N4 107.1(2)
C14 N3 W1 132.8(2)
N4 N3 W1 120.00(18)
C12 N4 N3 109.8(2)
C12 N4 B1 130.0(3)
N3 N4 B1 119.9(2)
C19 N5 N6 107.0(2)
C19 N5 W1 132.9(2)
N6 N5 W1 120.04(16)
C17 N6 N5 109.1(2)
C17 N6 B1 130.7(2)
N5 N6 B1 120.2(2)
O1 C1 W1 174.2(3)
C4 C3 C2 143.8(3)
C4 C3 W1 73.06(19)
C2 C3 W1 143.1(2)
C3 C4 C5 144.2(3)
C3 C4 W1 70.40(19)
C5 C4 W1 145.4(2)
N2 C7 C8 107.1(3)
N2 C7 C6 122.9(3)
C8 C7 C6 129.9(3)
C9 C8 C7 107.5(3)
N1 C9 C8 108.9(3)
N1 C9 C10 124.1(3)
C8 C9 C10 127.0(3)
N4 C12 C13 107.4(3)
N4 C12 C11 122.3(3)
C13 C12 C11 130.3(3)
C12 C13 C14 107.0(3)
N3 C14 C13 108.6(3)
N3 C14 C15 124.4(3)
C13 C14 C15 127.0(3)
N6 C17 C18 108.2(3)
N6 C17 C16 122.8(3)
C18 C17 C16 129.0(3)
C17 C18 C19 107.0(3)
N5 C19 C18 108.7(3)
N5 C19 C20 123.9(3)
C18 C19 C20 127.3(3)
N4 B1 N2 108.2(2)
N4 B1 N6 109.1(2)
N2 B1 N6 108.4(2)
F1 B2 F2 109.4(3)
F1 B2 F3 110.4(3)
F2 B2 F3 109.2(3)
F1 B2 F4 109.5(3)
F2 B2 F4 108.4(3)
F3 B2 F4 110.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 C3 2.035(3)
W1 C4 2.067(3)
W1 C1 2.087(3)
W1 N5 2.146(2)
W1 N3 2.175(2)
W1 N1 2.216(2)
W1 Cl1 2.3429(8)
O1 C1 1.114(4)
N1 C9 1.360(3)
N1 N2 1.379(3)
N2 C7 1.354(4)
N2 B1 1.531(4)
N3 C14 1.352(4)
N3 N4 1.375(3)
N4 C12 1.346(4)
N4 B1 1.528(4)
N5 C19 1.360(3)
N5 N6 1.384(3)
N6 C17 1.348(4)
N6 B1 1.543(4)
C2 C3 1.477(4)
C3 C4 1.286(4)
C4 C5 1.484(4)
C6 C7 1.494(4)
C7 C8 1.381(4)
C8 C9 1.380(4)
C9 C10 1.500(4)
C11 C12 1.484(4)
C12 C13 1.384(4)
C13 C14 1.389(4)
C14 C15 1.488(4)
C16 C17 1.502(4)
C17 C18 1.379(4)
C18 C19 1.385(4)
C19 C20 1.487(4)
B2 F1 1.378(4)
B2 F2 1.383(4)
B2 F3 1.384(4)
B2 F4 1.385(4)
