#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:12:39 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179681 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/03/7000327.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_7000327
loop_
_publ_author_name
'Adams, Christopher J.'
'Anderson, Kirsty M.'
'Connelly, Neil G.'
'Harding, David J.'
'Hayward, Owen D.'
'Orpen, A. Guy'
'Patrón, Elena'
'Rieger, Philip H.'
_publ_section_title
;
 The d3/d2 alkyne complexes [MX2(η-RCCR)Tp′]z (X =
 halide, z = 0 and 1+): final links in a d6--d2 redox family tree
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              530
_journal_page_last               543
_journal_paper_doi               10.1039/b813642d
_journal_year                    2009
_chemical_formula_sum            'C29 H32 B Cl7 F N6 Sb W'
_chemical_formula_weight         1048.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 102.369(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5069(18)
_cell_length_b                   16.1788(15)
_cell_length_c                   19.1244(15)
_cell_measurement_temperature    173(2)
_cell_volume                     4082.2(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans 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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45157
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.968
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red-brown
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0296P)²+5.8950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                8183
_reflns_number_total             9360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813642d.txt
_cod_data_source_block           3[SbCl6]
_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)/c
_cod_database_code               7000327
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 1.432631(9) 0.924039(7) 0.268067(6) 0.01437(4) Uani 1 1 d . . .
F1 F 1.36193(14) 1.02592(11) 0.27261(10) 0.0233(4) Uani 1 1 d . . .
Cl1 Cl 1.43705(7) 0.86822(5) 0.38022(4) 0.02816(18) Uani 1 1 d . . .
N1 N 1.5601(2) 1.00013(16) 0.32508(14) 0.0209(6) Uani 1 1 d . . .
N2 N 1.6513(2) 0.99943(16) 0.30407(14) 0.0211(6) Uani 1 1 d . . .
C1 C 1.4863(3) 1.0728(2) 0.4182(2) 0.0377(9) Uani 1 1 d . . .
H1A H 1.4252 1.0421 0.3958 0.057 Uiso 1 1 calc R . .
H1B H 1.4729 1.1323 0.4128 0.057 Uiso 1 1 calc R . .
H1C H 1.5052 1.0589 0.4692 0.057 Uiso 1 1 calc R . .
C2 C 1.5707(3) 1.0504(2) 0.38291(18) 0.0274(8) Uani 1 1 d . . .
C3 C 1.6697(3) 1.0795(2) 0.3992(2) 0.0342(9) Uani 1 1 d . . .
H3A H 1.6982 1.1154 0.4375 0.041 Uiso 1 1 calc R . .
C4 C 1.7192(3) 1.0468(2) 0.34972(19) 0.0287(8) Uani 1 1 d . . .
C5 C 1.8271(3) 1.0559(3) 0.3431(2) 0.0435(10) Uani 1 1 d . . .
H5A H 1.8378 1.0244 0.3016 0.065 Uiso 1 1 calc R . .
H5B H 1.8721 1.0349 0.3866 0.065 Uiso 1 1 calc R . .
H5C H 1.8418 1.1144 0.3368 0.065 Uiso 1 1 calc R . .
N3 N 1.47586(19) 0.98013(15) 0.17754(13) 0.0174(5) Uani 1 1 d . . .
N4 N 1.57652(19) 0.98434(15) 0.17460(13) 0.0177(5) Uani 1 1 d . . .
C6 C 1.3098(3) 1.0300(2) 0.10398(18) 0.0282(8) Uani 1 1 d . . .
H6A H 1.2825 1.0030 0.1417 0.042 Uiso 1 1 calc R . .
H6B H 1.2796 1.0051 0.0576 0.042 Uiso 1 1 calc R . .
H6C H 1.2937 1.0891 0.1028 0.042 Uiso 1 1 calc R . .
C7 C 1.4218(3) 1.01896(19) 0.11884(16) 0.0210(7) Uani 1 1 d . . .
C8 C 1.4888(3) 1.0474(2) 0.07843(17) 0.0254(7) Uani 1 1 d . . .
H8A H 1.4717 1.0772 0.0347 0.030 Uiso 1 1 calc R . .
C9 C 1.5850(3) 1.0242(2) 0.11383(17) 0.0229(7) Uani 1 1 d . . .
C10 C 1.6842(3) 1.0381(2) 0.0940(2) 0.0348(9) Uani 1 1 d . . .
H10A H 1.7383 1.0137 0.1306 0.052 Uiso 1 1 calc R . .
H10B H 1.6960 1.0976 0.0908 0.052 Uiso 1 1 calc R . .
H10C H 1.6836 1.0121 0.0476 0.052 Uiso 1 1 calc R . .
N5 N 1.5427(2) 0.83598(15) 0.25604(13) 0.0180(5) Uani 1 1 d . . .
N6 N 1.63784(19) 0.86008(16) 0.24873(13) 0.0191(5) Uani 1 1 d . . .
C11 C 1.4567(3) 0.7001(2) 0.2699(2) 0.0298(8) Uani 1 1 d . . .
H11A H 1.3983 0.7359 0.2700 0.045 Uiso 1 1 calc R . .
H11B H 1.4743 0.6699 0.3153 0.045 Uiso 1 1 calc R . .
H11C H 1.4398 0.6606 0.2302 0.045 Uiso 1 1 calc R . .
C12 C 1.5445(3) 0.75128(19) 0.26081(17) 0.0213(7) Uani 1 1 d . . .
C13 C 1.6399(3) 0.7242(2) 0.25724(18) 0.0277(8) Uani 1 1 d . . .
H13A H 1.6624 0.6685 0.2593 0.033 Uiso 1 1 calc R . .
C14 C 1.6969(3) 0.7936(2) 0.25016(17) 0.0233(7) Uani 1 1 d . . .
C15 C 1.8072(3) 0.7993(2) 0.2475(2) 0.0344(9) Uani 1 1 d . . .
H15A H 1.8254 0.8573 0.2425 0.052 Uiso 1 1 calc R . .
H15B H 1.8194 0.7676 0.2064 0.052 Uiso 1 1 calc R . .
H15C H 1.8486 0.7766 0.2917 0.052 Uiso 1 1 calc R . .
B1 B 1.6602(3) 0.9518(2) 0.23673(19) 0.0203(7) Uani 1 1 d . . .
H1 H 1.7290 0.9589 0.2259 0.024 Uiso 1 1 calc R . .
C16 C 1.3386(2) 0.85543(18) 0.19233(16) 0.0165(6) Uani 1 1 d . . .
C17 C 1.2945(2) 0.86795(18) 0.24601(16) 0.0183(6) Uani 1 1 d . . .
C18 C 1.2116(2) 0.8511(2) 0.28062(17) 0.0231(7) Uani 1 1 d . . .
C19 C 1.1904(3) 0.9049(2) 0.33244(19) 0.0304(8) Uani 1 1 d . . .
H19A H 1.2297 0.9536 0.3443 0.037 Uiso 1 1 calc R . .
C20 C 1.1122(3) 0.8877(3) 0.3668(2) 0.0435(10) Uani 1 1 d . . .
H20A H 1.0966 0.9254 0.4009 0.052 Uiso 1 1 calc R . .
C21 C 1.0575(3) 0.8164(3) 0.3513(2) 0.0507(13) Uani 1 1 d . . .
H21A H 1.0049 0.8044 0.3758 0.061 Uiso 1 1 calc R . .
C22 C 1.0774(3) 0.7612(3) 0.3006(2) 0.0496(12) Uani 1 1 d . . .
H22A H 1.0394 0.7115 0.2910 0.059 Uiso 1 1 calc R . .
C23 C 1.1539(3) 0.7793(3) 0.26354(19) 0.0335(9) Uani 1 1 d . . .
H23A H 1.1664 0.7431 0.2273 0.040 Uiso 1 1 calc R . .
C24 C 1.3251(2) 0.82052(19) 0.12087(16) 0.0190(6) Uani 1 1 d . . .
C25 C 1.2273(3) 0.8000(2) 0.08411(17) 0.0233(7) Uani 1 1 d . . .
H25A H 1.1718 0.8066 0.1069 0.028 Uiso 1 1 calc R . .
C26 C 1.2105(3) 0.7702(2) 0.01450(18) 0.0291(8) Uani 1 1 d . . .
H26A H 1.1436 0.7578 -0.0107 0.035 Uiso 1 1 calc R . .
C27 C 1.2918(3) 0.7586(2) -0.01815(17) 0.0302(8) Uani 1 1 d . . .
H27A H 1.2806 0.7377 -0.0656 0.036 Uiso 1 1 calc R . .
C28 C 1.3894(3) 0.7772(2) 0.01822(18) 0.0284(8) Uani 1 1 d . . .
H28A H 1.4449 0.7685 -0.0042 0.034 Uiso 1 1 calc R . .
C29 C 1.4064(3) 0.80875(19) 0.08734(17) 0.0222(7) Uani 1 1 d . . .
H29A H 1.4733 0.8223 0.1118 0.027 Uiso 1 1 calc R . .
Sb1 Sb 0.826741(17) 0.794548(14) 0.525125(12) 0.02298(6) Uani 1 1 d . . .
Cl2 Cl 0.71293(8) 0.69219(7) 0.55206(6) 0.0441(2) Uani 1 1 d . . .
Cl3 Cl 0.86588(11) 0.70681(7) 0.43558(6) 0.0557(3) Uani 1 1 d . . .
Cl4 Cl 0.96062(8) 0.73326(9) 0.60892(6) 0.0582(3) Uani 1 1 d . . .
Cl5 Cl 0.69405(10) 0.85256(10) 0.44104(7) 0.0730(4) Uani 1 1 d . . .
Cl6 Cl 0.79029(11) 0.87770(7) 0.61691(7) 0.0572(3) Uani 1 1 d . . .
Cl7 Cl 0.94101(10) 0.89547(8) 0.49915(6) 0.0539(3) 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'
Cl Cl 0.1484 0.1585 '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
F1 W1 C17 87.10(10) . . ?
F1 W1 C16 105.07(10) . . ?
C17 W1 C16 37.47(12) . . ?
F1 W1 N5 163.09(9) . . ?
C17 W1 N5 108.20(11) . . ?
C16 W1 N5 84.30(11) . . ?
F1 W1 N3 84.09(9) . . ?
C17 W1 N3 114.67(11) . . ?
C16 W1 N3 83.83(11) . . ?
N5 W1 N3 82.97(10) . . ?
F1 W1 N1 80.87(9) . . ?
C17 W1 N1 159.22(11) . . ?
C16 W1 N1 163.08(11) . . ?
N5 W1 N1 86.40(10) . . ?
N3 W1 N1 81.03(10) . . ?
F1 W1 Cl1 101.98(6) . . ?
C17 W1 Cl1 81.88(9) . . ?
C16 W1 Cl1 109.54(9) . . ?
N5 W1 Cl1 87.63(7) . . ?
N3 W1 Cl1 162.85(7) . . ?
N1 W1 Cl1 84.11(7) . . ?
C2 N1 N2 107.4(3) . . ?
C2 N1 W1 132.3(2) . . ?
N2 N1 W1 120.29(19) . . ?
C4 N2 N1 109.3(3) . . ?
C4 N2 B1 131.5(3) . . ?
N1 N2 B1 119.2(2) . . ?
N1 C2 C3 108.3(3) . . ?
N1 C2 C1 124.0(3) . . ?
C3 C2 C1 127.6(3) . . ?
C4 C3 C2 107.6(3) . . ?
N2 C4 C3 107.4(3) . . ?
N2 C4 C5 122.4(3) . . ?
C3 C4 C5 130.2(3) . . ?
C7 N3 N4 107.8(2) . . ?
C7 N3 W1 132.3(2) . . ?
N4 N3 W1 119.80(18) . . ?
C9 N4 N3 109.0(2) . . ?
C9 N4 B1 129.7(3) . . ?
N3 N4 B1 121.2(2) . . ?
N3 C7 C8 108.3(3) . . ?
N3 C7 C6 124.0(3) . . ?
C8 C7 C6 127.6(3) . . ?
C9 C8 C7 107.1(3) . . ?
N4 C9 C8 107.8(3) . . ?
N4 C9 C10 122.5(3) . . ?
C8 C9 C10 129.7(3) . . ?
C12 N5 N6 106.6(3) . . ?
C12 N5 W1 132.1(2) . . ?
N6 N5 W1 120.98(19) . . ?
C14 N6 N5 109.6(3) . . ?
C14 N6 B1 130.0(3) . . ?
N5 N6 B1 120.3(2) . . ?
N5 C12 C13 108.5(3) . . ?
N5 C12 C11 124.1(3) . . ?
C13 C12 C11 127.4(3) . . ?
C12 C13 C14 107.1(3) . . ?
N6 C14 C13 108.2(3) . . ?
N6 C14 C15 122.8(3) . . ?
C13 C14 C15 129.0(3) . . ?
N2 B1 N6 107.8(3) . . ?
N2 B1 N4 107.5(3) . . ?
N6 B1 N4 107.9(2) . . ?
C17 C16 C24 144.2(3) . . ?
C17 C16 W1 71.15(19) . . ?
C24 C16 W1 144.5(2) . . ?
C16 C17 C18 149.2(3) . . ?
C16 C17 W1 71.38(19) . . ?
C18 C17 W1 139.1(2) . . ?
C19 C18 C23 119.8(3) . . ?
C19 C18 C17 120.4(3) . . ?
C23 C18 C17 119.8(3) . . ?
C20 C19 C18 120.3(4) . . ?
C21 C20 C19 119.9(4) . . ?
C20 C21 C22 121.1(4) . . ?
C21 C22 C23 119.6(4) . . ?
C18 C23 C22 119.2(4) . . ?
C25 C24 C29 119.2(3) . . ?
C25 C24 C16 118.7(3) . . ?
C29 C24 C16 122.0(3) . . ?
C26 C25 C24 120.5(3) . . ?
C27 C26 C25 119.8(3) . . ?
C28 C27 C26 120.3(3) . . ?
C27 C28 C29 120.2(3) . . ?
C28 C29 C24 120.0(3) . . ?
Cl5 Sb1 Cl6 91.82(6) . . ?
Cl5 Sb1 Cl4 178.83(6) . . ?
Cl6 Sb1 Cl4 89.20(5) . . ?
Cl5 Sb1 Cl3 90.01(6) . . ?
Cl6 Sb1 Cl3 177.91(5) . . ?
Cl4 Sb1 Cl3 88.97(5) . . ?
Cl5 Sb1 Cl7 90.97(5) . . ?
Cl6 Sb1 Cl7 90.70(4) . . ?
Cl4 Sb1 Cl7 89.60(5) . . ?
Cl3 Sb1 Cl7 90.29(4) . . ?
Cl5 Sb1 Cl2 89.58(5) . . ?
Cl6 Sb1 Cl2 89.33(4) . . ?
Cl4 Sb1 Cl2 89.84(4) . . ?
Cl3 Sb1 Cl2 89.66(4) . . ?
Cl7 Sb1 Cl2 179.44(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 F1 1.9162(18) . ?
W1 C17 2.035(3) . ?
W1 C16 2.038(3) . ?
W1 N5 2.107(3) . ?
W1 N3 2.144(2) . ?
W1 N1 2.206(3) . ?
W1 Cl1 2.3161(8) . ?
N1 C2 1.356(4) . ?
N1 N2 1.375(4) . ?
N2 C4 1.359(4) . ?
N2 B1 1.527(5) . ?
C1 C2 1.489(6) . ?
C2 C3 1.389(5) . ?
C3 C4 1.375(6) . ?
C4 C5 1.496(6) . ?
N3 C7 1.355(4) . ?
N3 N4 1.374(4) . ?
N4 C9 1.356(4) . ?
N4 B1 1.546(4) . ?
C6 C7 1.488(5) . ?
C7 C8 1.388(5) . ?
C8 C9 1.383(5) . ?
C9 C10 1.484(5) . ?
N5 C12 1.373(4) . ?
N5 N6 1.379(4) . ?
N6 C14 1.336(4) . ?
N6 B1 1.542(4) . ?
C11 C12 1.486(5) . ?
C12 C13 1.377(5) . ?
C13 C14 1.383(5) . ?
C14 C15 1.504(5) . ?
C16 C17 1.308(4) . ?
C16 C24 1.453(4) . ?
C17 C18 1.444(4) . ?
C18 C19 1.394(5) . ?
C18 C23 1.398(5) . ?
C19 C20 1.386(5) . ?
C20 C21 1.368(7) . ?
C21 C22 1.386(7) . ?
C22 C23 1.404(6) . ?
C24 C25 1.397(4) . ?
C24 C29 1.399(5) . ?
C25 C26 1.388(5) . ?
C26 C27 1.388(5) . ?
C27 C28 1.385(5) . ?
C28 C29 1.389(4) . ?
Sb1 Cl5 2.3333(11) . ?
Sb1 Cl6 2.3460(11) . ?
Sb1 Cl4 2.3621(10) . ?
Sb1 Cl3 2.3696(11) . ?
Sb1 Cl7 2.3714(11) . ?
Sb1 Cl2 2.3896(10) . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 263.6 98.7
2 0.000 0.500 0.500 263.6 98.1
