#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:31:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179752 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/48/7004842.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_7004842
loop_
_publ_author_name
'Adams, Christopher J.'
'Bartlett, Ian M.'
'Carlton, Susannah'
'Connelly, Neil G.'
'Harding, David J.'
'Hayward, Owen D.'
'Orpen, A. Guy'
'Patron, Elena'
'Ray, Christopher D.'
'Rieger, Philip H.'
_publ_section_title
;
 The d4/d3 redox pairs [MX(CO)(eta-RC[triple bond, length as
 m-dash]CR)Tp']z (z=0 and 1): structural consequences of electron
 transfer and implications for the inverse halide order.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              62
_journal_page_last               72
_journal_paper_doi               10.1039/b611472e
_journal_year                    2007
_chemical_formula_sum            'C20 H28 B Cl N6 O W'
_chemical_formula_weight         598.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 116.552(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   18.243(4)
_cell_length_b                   10.0941(16)
_cell_length_c                   14.0120(15)
_cell_measurement_reflns_used    113
_cell_measurement_temperature    173(2)
_cell_volume                     2308.1(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD 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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11755
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.144
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.047(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5159
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0265
_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)+(0.0114P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0457
_reflns_number_gt                4476
_reflns_number_total             5159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b611472e.txt
_cod_data_source_block           11
_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      Cc
_cod_database_code               7004842
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, 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 0.483350(15) 0.162827(17) 0.013450(16) 0.01697(5) Uani 1 1 d . . .
Cl1 Cl 0.50242(8) 0.40149(12) 0.02226(19) 0.0283(4) Uani 1 1 d . . .
O1 O 0.6389(2) 0.1092(4) -0.0187(3) 0.0344(10) Uani 1 1 d . . .
N1 N 0.4367(3) -0.0387(4) -0.0336(3) 0.0194(10) Uani 1 1 d . . .
N2 N 0.3553(3) -0.0637(4) -0.1007(3) 0.0216(10) Uani 1 1 d . . .
N3 N 0.3592(3) 0.2082(5) 0.0023(4) 0.0199(10) Uani 1 1 d . . .
N4 N 0.2912(2) 0.1437(4) -0.0743(3) 0.0216(10) Uani 1 1 d . . .
N5 N 0.4140(3) 0.1894(4) -0.1630(4) 0.0222(11) Uani 1 1 d . . .
N6 N 0.3366(3) 0.1301(4) -0.2174(4) 0.0223(11) Uani 1 1 d . . .
C1 C 0.5797(3) 0.1325(5) -0.0086(4) 0.0219(13) Uani 1 1 d . . .
C2 C 0.6715(4) 0.0919(7) 0.2203(5) 0.0306(18) Uani 1 1 d . . .
H2A H 0.7009 0.1743 0.2233 0.046 Uiso 1 1 calc R . .
H2B H 0.6892 0.0227 0.1860 0.046 Uiso 1 1 calc R . .
H2C H 0.6836 0.0640 0.2928 0.046 Uiso 1 1 calc R . .
C3 C 0.5800(4) 0.1145(5) 0.1564(5) 0.0256(13) Uani 1 1 d . . .
C4 C 0.5126(3) 0.1193(5) 0.1656(5) 0.0252(14) Uani 1 1 d . . .
C5 C 0.4817(4) 0.0872(6) 0.2458(5) 0.0359(15) Uani 1 1 d . . .
H5A H 0.4566 -0.0010 0.2309 0.054 Uiso 1 1 calc R . .
H5B H 0.4409 0.1532 0.2413 0.054 Uiso 1 1 calc R . .
H5C H 0.5276 0.0884 0.3177 0.054 Uiso 1 1 calc R . .
C6 C 0.5606(4) -0.1839(6) 0.0696(5) 0.0318(15) Uani 1 1 d . . .
H6A H 0.5734 -0.2785 0.0715 0.048 Uiso 1 1 calc R . .
H6B H 0.5710 -0.1544 0.1411 0.048 Uiso 1 1 calc R . .
H6C H 0.5952 -0.1335 0.0456 0.048 Uiso 1 1 calc R . .
C7 C 0.4723(5) -0.1615(5) -0.0062(5) 0.0166(15) Uani 1 1 d . . .
C8 C 0.4154(4) -0.2598(6) -0.0575(5) 0.0284(15) Uani 1 1 d . . .
H8 H 0.4245 -0.3527 -0.0528 0.034 Uiso 1 1 calc R . .
C9 C 0.3427(4) -0.1948(5) -0.1168(4) 0.0259(14) Uani 1 1 d . . .
C10 C 0.2599(4) -0.2530(6) -0.1864(5) 0.0413(17) Uani 1 1 d . . .
H10A H 0.2215 -0.2293 -0.1578 0.062 Uiso 1 1 calc R . .
H10B H 0.2644 -0.3496 -0.1878 0.062 Uiso 1 1 calc R . .
H10C H 0.2398 -0.2180 -0.2590 0.062 Uiso 1 1 calc R . .
C11 C 0.3857(4) 0.3784(6) 0.1456(5) 0.0375(16) Uani 1 1 d . . .
H11A H 0.3696 0.3734 0.2035 0.056 Uiso 1 1 calc R . .
H11B H 0.3799 0.4699 0.1196 0.056 Uiso 1 1 calc R . .
H11C H 0.4428 0.3503 0.1720 0.056 Uiso 1 1 calc R . .
C12 C 0.3311(3) 0.2886(5) 0.0554(5) 0.0265(13) Uani 1 1 d . . .
C13 C 0.2468(3) 0.2757(5) 0.0150(5) 0.0295(14) Uani 1 1 d . . .
H13 H 0.2126 0.3215 0.0388 0.035 Uiso 1 1 calc R . .
C14 C 0.2222(3) 0.1839(5) -0.0660(4) 0.0256(13) Uani 1 1 d . . .
C15 C 0.1387(3) 0.1279(6) -0.1346(5) 0.0357(16) Uani 1 1 d . . .
H15A H 0.0997 0.1614 -0.1100 0.054 Uiso 1 1 calc R . .
H15B H 0.1409 0.0310 -0.1297 0.054 Uiso 1 1 calc R . .
H15C H 0.1211 0.1547 -0.2089 0.054 Uiso 1 1 calc R . .
C16 C 0.5066(4) 0.3225(6) -0.2139(5) 0.0408(16) Uani 1 1 d . . .
H16A H 0.5012 0.3700 -0.2778 0.061 Uiso 1 1 calc R . .
H16B H 0.5528 0.2606 -0.1910 0.061 Uiso 1 1 calc R . .
H16C H 0.5165 0.3863 -0.1567 0.061 Uiso 1 1 calc R . .
C17 C 0.4304(3) 0.2483(5) -0.2386(4) 0.0245(13) Uani 1 1 d . . .
C18 C 0.3645(4) 0.2297(6) -0.3375(5) 0.0296(14) Uani 1 1 d . . .
H18 H 0.3596 0.2631 -0.4035 0.036 Uiso 1 1 calc R . .
C19 C 0.3069(3) 0.1542(6) -0.3234(4) 0.0245(12) Uani 1 1 d . . .
C20 C 0.2282(4) 0.0977(6) -0.4049(5) 0.0334(15) Uani 1 1 d . . .
H20A H 0.2165 0.1332 -0.4754 0.050 Uiso 1 1 calc R . .
H20B H 0.1838 0.1218 -0.3871 0.050 Uiso 1 1 calc R . .
H20C H 0.2327 0.0010 -0.4058 0.050 Uiso 1 1 calc R . .
B1 B 0.2986(5) 0.0536(8) -0.1563(6) 0.0253(19) Uani 1 1 d . . .
H1 H 0.237(3) 0.020(4) -0.218(4) 0.009(12) Uiso 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W1 C4 107.8(2) . . ?
C1 W1 C3 70.9(2) . . ?
C4 W1 C3 37.3(2) . . ?
C1 W1 N1 93.6(2) . . ?
C4 W1 N1 89.95(19) . . ?
C3 W1 N1 96.98(18) . . ?
C1 W1 N5 87.0(2) . . ?
C4 W1 N5 162.71(19) . . ?
C3 W1 N5 157.53(19) . . ?
N1 W1 N5 80.02(16) . . ?
C1 W1 N3 168.0(2) . . ?
C4 W1 N3 84.2(2) . . ?
C3 W1 N3 121.1(2) . . ?
N1 W1 N3 85.69(16) . . ?
N5 W1 N3 81.04(16) . . ?
C1 W1 Cl1 92.59(16) . . ?
C4 W1 Cl1 101.53(16) . . ?
C3 W1 Cl1 98.36(15) . . ?
N1 W1 Cl1 164.61(11) . . ?
N5 W1 Cl1 86.26(12) . . ?
N3 W1 Cl1 85.31(12) . . ?
C7 N1 N2 104.8(4) . . ?
C7 N1 W1 133.2(4) . . ?
N2 N1 W1 122.0(3) . . ?
C9 N2 N1 110.2(4) . . ?
C9 N2 B1 130.4(5) . . ?
N1 N2 B1 118.7(4) . . ?
C12 N3 N4 106.2(4) . . ?
C12 N3 W1 134.8(4) . . ?
N4 N3 W1 119.0(3) . . ?
C14 N4 N3 109.4(4) . . ?
C14 N4 B1 129.4(5) . . ?
N3 N4 B1 120.9(5) . . ?
C17 N5 N6 106.4(4) . . ?
C17 N5 W1 134.6(4) . . ?
N6 N5 W1 118.9(3) . . ?
C19 N6 N5 109.2(5) . . ?
C19 N6 B1 130.2(5) . . ?
N5 N6 B1 120.6(5) . . ?
O1 C1 W1 176.9(5) . . ?
C4 C3 C2 142.2(6) . . ?
C4 C3 W1 69.4(4) . . ?
C2 C3 W1 148.3(5) . . ?
C3 C4 C5 139.3(6) . . ?
C3 C4 W1 73.4(4) . . ?
C5 C4 W1 146.6(4) . . ?
N1 C7 C8 110.6(6) . . ?
N1 C7 C6 123.9(5) . . ?
C8 C7 C6 125.5(6) . . ?
C9 C8 C7 105.6(5) . . ?
N2 C9 C8 108.7(5) . . ?
N2 C9 C10 122.7(5) . . ?
C8 C9 C10 128.5(5) . . ?
N3 C12 C13 110.1(5) . . ?
N3 C12 C11 123.5(5) . . ?
C13 C12 C11 126.4(5) . . ?
C14 C13 C12 107.1(5) . . ?
C13 C14 N4 107.1(5) . . ?
C13 C14 C15 130.3(5) . . ?
N4 C14 C15 122.6(5) . . ?
N5 C17 C18 109.0(5) . . ?
N5 C17 C16 123.5(5) . . ?
C18 C17 C16 127.5(5) . . ?
C19 C18 C17 107.9(5) . . ?
N6 C19 C18 107.4(5) . . ?
N6 C19 C20 123.1(5) . . ?
C18 C19 C20 129.4(5) . . ?
N4 B1 N6 109.8(6) . . ?
N4 B1 N2 110.2(5) . . ?
N6 B1 N2 107.6(6) . . ?
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 C1 1.941(6) . ?
W1 C4 2.002(6) . ?
W1 C3 2.050(6) . ?
W1 N1 2.190(4) . ?
W1 N5 2.234(5) . ?
W1 N3 2.246(5) . ?
W1 Cl1 2.4293(13) . ?
O1 C1 1.174(6) . ?
N1 C7 1.372(6) . ?
N1 N2 1.381(5) . ?
N2 C9 1.344(6) . ?
N2 B1 1.536(9) . ?
N3 C12 1.348(7) . ?
N3 N4 1.388(6) . ?
N4 C14 1.376(6) . ?
N4 B1 1.519(10) . ?
N5 C17 1.359(7) . ?
N5 N6 1.405(6) . ?
N6 C19 1.357(6) . ?
N6 B1 1.528(9) . ?
C2 C3 1.518(9) . ?
C3 C4 1.295(8) . ?
C4 C5 1.499(8) . ?
C6 C7 1.499(9) . ?
C7 C8 1.382(8) . ?
C8 C9 1.376(8) . ?
C9 C10 1.504(8) . ?
C11 C12 1.511(7) . ?
C12 C13 1.388(8) . ?
C13 C14 1.375(8) . ?
C14 C15 1.501(7) . ?
C16 C17 1.478(7) . ?
C17 C18 1.383(7) . ?
C18 C19 1.382(8) . ?
C19 C20 1.491(7) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C4 C1 O1 15.1(8) . . . . ?
