#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:12:39 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179681 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/03/7000330.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_7000330
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 F2 N6 W'
_chemical_formula_weight         697.27
_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                 113.989(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6427(17)
_cell_length_b                   32.628(7)
_cell_length_c                   9.8228(17)
_cell_measurement_reflns_used    123
_cell_measurement_temperature    173(2)
_cell_volume                     2823.5(10)
_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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29564
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.134
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            Magenta
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.662
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0294
_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)+(0.0250P)²+0.9972P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                4725
_reflns_number_total             6494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813642d.txt
_cod_data_source_block           2
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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_cell_volume        2823.6(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7000330
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 -0.405019(17) 0.124971(5) -0.380783(17) 0.01906(5) Uani 1 1 d . . .
F1 F -0.2193(2) 0.09308(7) -0.3080(3) 0.0270(5) Uani 1 1 d . . .
F2 F -0.3250(3) 0.15847(7) -0.1966(2) 0.0266(5) Uani 1 1 d . . .
N1 N -0.4673(4) 0.08479(10) -0.2279(4) 0.0210(7) Uani 1 1 d . . .
N2 N -0.6129(4) 0.07022(10) -0.2738(4) 0.0216(7) Uani 1 1 d . . .
C1 C -0.2325(5) 0.08544(16) 0.0077(5) 0.0362(12) Uani 1 1 d . . .
H1A H -0.1730 0.0797 -0.0506 0.054 Uiso 1 1 calc R . .
H1B H -0.1938 0.0689 0.0990 0.054 Uiso 1 1 calc R . .
H1C H -0.2240 0.1146 0.0338 0.054 Uiso 1 1 calc R . .
C2 C -0.3951(5) 0.07494(13) -0.0823(5) 0.0249(9) Uani 1 1 d . . .
C3 C -0.4949(5) 0.05433(13) -0.0364(5) 0.0292(10) Uani 1 1 d . . .
H3A H -0.4730 0.0436 0.0601 0.035 Uiso 1 1 calc R . .
C4 C -0.6317(5) 0.05254(13) -0.1585(5) 0.0255(10) Uani 1 1 d . . .
C5 C -0.7805(5) 0.03598(15) -0.1683(5) 0.0355(11) Uani 1 1 d . . .
H5A H -0.8229 0.0174 -0.2537 0.053 Uiso 1 1 calc R . .
H5B H -0.8512 0.0587 -0.1811 0.053 Uiso 1 1 calc R . .
H5C H -0.7648 0.0211 -0.0766 0.053 Uiso 1 1 calc R . .
N3 N -0.5127(3) 0.07341(10) -0.5255(4) 0.0201(7) Uani 1 1 d . . .
N4 N -0.6541(4) 0.05970(10) -0.5407(4) 0.0218(7) Uani 1 1 d . . .
C6 C -0.3251(5) 0.05770(14) -0.6314(5) 0.0299(10) Uani 1 1 d . . .
H6A H -0.2462 0.0643 -0.5330 0.045 Uiso 1 1 calc R . .
H6B H -0.3356 0.0805 -0.7000 0.045 Uiso 1 1 calc R . .
H6C H -0.2968 0.0328 -0.6695 0.045 Uiso 1 1 calc R . .
C7 C -0.4733(5) 0.05097(13) -0.6185(4) 0.0240(9) Uani 1 1 d . . .
C8 C -0.5871(5) 0.02282(13) -0.6931(4) 0.0261(9) Uani 1 1 d . . .
H8A H -0.5873 0.0031 -0.7644 0.031 Uiso 1 1 calc R . .
C9 C -0.6999(5) 0.02918(12) -0.6429(5) 0.0246(9) Uani 1 1 d . . .
C10 C -0.8500(5) 0.00840(14) -0.6907(5) 0.0346(11) Uani 1 1 d . . .
H10A H -0.8679 0.0008 -0.6027 0.052 Uiso 1 1 calc R . .
H10B H -0.8506 -0.0163 -0.7477 0.052 Uiso 1 1 calc R . .
H10C H -0.9303 0.0270 -0.7533 0.052 Uiso 1 1 calc R . .
N5 N -0.6255(4) 0.14930(10) -0.4187(4) 0.0210(7) Uani 1 1 d . . .
N6 N -0.7485(3) 0.12351(11) -0.4607(3) 0.0222(7) Uani 1 1 d . . .
C11 C -0.5770(5) 0.22449(14) -0.3948(6) 0.0385(12) Uani 1 1 d . . .
H11A H -0.4782 0.2178 -0.3153 0.058 Uiso 1 1 calc R . .
H11B H -0.6228 0.2473 -0.3626 0.058 Uiso 1 1 calc R . .
H11C H -0.5632 0.2325 -0.4847 0.058 Uiso 1 1 calc R . .
C12 C -0.6784(5) 0.18799(13) -0.4277(5) 0.0248(9) Uani 1 1 d . . .
C13 C -0.8347(5) 0.18690(14) -0.4766(5) 0.0281(10) Uani 1 1 d . . .
H13A H -0.9007 0.2098 -0.4941 0.034 Uiso 1 1 calc R . .
C14 C -0.8757(4) 0.14625(13) -0.4948(5) 0.0245(9) Uani 1 1 d . . .
C15 C -1.0300(5) 0.12735(16) -0.5447(5) 0.0363(11) Uani 1 1 d . . .
H15A H -1.0400 0.1053 -0.6157 0.054 Uiso 1 1 calc R . .
H15B H -1.1075 0.1483 -0.5929 0.054 Uiso 1 1 calc R . .
H15C H -1.0434 0.1162 -0.4583 0.054 Uiso 1 1 calc R . .
B1 B -0.7250(6) 0.07713(15) -0.4376(6) 0.0259(11) Uani 1 1 d . . .
H1 H -0.8239 0.0633 -0.4576 0.031 Uiso 1 1 calc R . .
C16 C -0.4307(4) 0.15221(12) -0.5776(5) 0.0219(9) Uani 1 1 d . . .
C17 C -0.3213(4) 0.17054(13) -0.4653(4) 0.0216(9) Uani 1 1 d . . .
C18 C -0.2126(5) 0.20451(13) -0.4200(5) 0.0232(9) Uani 1 1 d . . .
C19 C -0.0828(4) 0.20214(13) -0.2872(5) 0.0255(9) Uani 1 1 d . . .
H19A H -0.0650 0.1784 -0.2266 0.031 Uiso 1 1 calc R . .
C20 C 0.0198(5) 0.23401(14) -0.2432(5) 0.0288(11) Uani 1 1 d . . .
H20A H 0.1094 0.2317 -0.1542 0.035 Uiso 1 1 calc R . .
C21 C -0.0065(5) 0.26914(13) -0.3272(5) 0.0311(10) Uani 1 1 d . . .
H21A H 0.0646 0.2910 -0.2956 0.037 Uiso 1 1 calc R . .
C22 C -0.1370(5) 0.27278(14) -0.4584(5) 0.0333(11) Uani 1 1 d . . .
H22A H -0.1569 0.2974 -0.5149 0.040 Uiso 1 1 calc R . .
C23 C -0.2376(5) 0.24021(14) -0.5059(5) 0.0287(10) Uani 1 1 d . . .
H23A H -0.3243 0.2421 -0.5977 0.034 Uiso 1 1 calc R . .
C24 C -0.5157(5) 0.15322(13) -0.7393(4) 0.0231(9) Uani 1 1 d . . .
C25 C -0.4496(5) 0.16723(13) -0.8331(5) 0.0288(10) Uani 1 1 d . . .
H25A H -0.3484 0.1773 -0.7914 0.035 Uiso 1 1 calc R . .
C26 C -0.5299(6) 0.16671(14) -0.9867(5) 0.0358(11) Uani 1 1 d . . .
H26A H -0.4823 0.1752 -1.0499 0.043 Uiso 1 1 calc R . .
C27 C -0.6775(6) 0.15395(16) -1.0467(5) 0.0400(12) Uani 1 1 d . . .
H27A H -0.7334 0.1544 -1.1517 0.048 Uiso 1 1 calc R . .
C28 C -0.7467(5) 0.14026(15) -0.9556(5) 0.0374(12) Uani 1 1 d . . .
H28A H -0.8497 0.1317 -0.9981 0.045 Uiso 1 1 calc R . .
C29 C -0.6653(5) 0.13924(13) -0.8035(5) 0.0299(10) Uani 1 1 d . . .
H29B H -0.7116 0.1289 -0.7416 0.036 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'
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'
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
F1 W1 F2 90.05(10) . . ?
F1 W1 C17 94.75(13) . . ?
F2 W1 C17 84.10(13) . . ?
F1 W1 C16 108.65(12) . . ?
F2 W1 C16 118.34(14) . . ?
C17 W1 C16 37.78(15) . . ?
F1 W1 N5 163.68(11) . . ?
F2 W1 N5 86.86(11) . . ?
C17 W1 N5 100.85(14) . . ?
C16 W1 N5 86.84(13) . . ?
F1 W1 N3 87.13(11) . . ?
F2 W1 N3 158.21(11) . . ?
C17 W1 N3 117.66(14) . . ?
C16 W1 N3 82.91(14) . . ?
N5 W1 N3 89.81(12) . . ?
F1 W1 N1 84.18(11) . . ?
F2 W1 N1 79.79(11) . . ?
C17 W1 N1 163.85(14) . . ?
C16 W1 N1 156.81(14) . . ?
N5 W1 N1 79.50(12) . . ?
N3 W1 N1 78.43(12) . . ?
C2 N1 N2 106.5(3) . . ?
C2 N1 W1 133.0(3) . . ?
N2 N1 W1 119.8(2) . . ?
C4 N2 N1 110.0(3) . . ?
C4 N2 B1 131.3(3) . . ?
N1 N2 B1 118.7(3) . . ?
N1 C2 C3 109.3(4) . . ?
N1 C2 C1 122.5(4) . . ?
C3 C2 C1 128.1(4) . . ?
C4 C3 C2 106.4(4) . . ?
N2 C4 C3 107.8(4) . . ?
N2 C4 C5 123.6(4) . . ?
C3 C4 C5 128.6(4) . . ?
C7 N3 N4 106.8(3) . . ?
C7 N3 W1 132.5(3) . . ?
N4 N3 W1 120.6(2) . . ?
C9 N4 N3 109.1(3) . . ?
C9 N4 B1 131.3(3) . . ?
N3 N4 B1 119.3(3) . . ?
N3 C7 C8 109.8(4) . . ?
N3 C7 C6 121.4(4) . . ?
C8 C7 C6 128.8(4) . . ?
C9 C8 C7 106.3(4) . . ?
N4 C9 C8 108.0(4) . . ?
N4 C9 C10 123.4(4) . . ?
C8 C9 C10 128.6(4) . . ?
C12 N5 N6 107.2(3) . . ?
C12 N5 W1 132.5(3) . . ?
N6 N5 W1 119.8(2) . . ?
C14 N6 N5 108.9(4) . . ?
C14 N6 B1 129.9(3) . . ?
N5 N6 B1 120.2(3) . . ?
N5 C12 C13 109.1(4) . . ?
N5 C12 C11 122.4(4) . . ?
C13 C12 C11 128.4(4) . . ?
C14 C13 C12 106.6(4) . . ?
N6 C14 C13 108.2(4) . . ?
N6 C14 C15 122.4(4) . . ?
C13 C14 C15 129.4(4) . . ?
N6 B1 N4 110.1(4) . . ?
N6 B1 N2 107.2(3) . . ?
N4 B1 N2 108.7(3) . . ?
C17 C16 C24 143.4(4) . . ?
C17 C16 W1 70.1(2) . . ?
C24 C16 W1 146.5(3) . . ?
C16 C17 C18 145.8(4) . . ?
C16 C17 W1 72.1(3) . . ?
C18 C17 W1 141.8(3) . . ?
C19 C18 C23 118.6(4) . . ?
C19 C18 C17 120.1(4) . . ?
C23 C18 C17 121.3(4) . . ?
C20 C19 C18 120.5(4) . . ?
C21 C20 C19 120.5(4) . . ?
C20 C21 C22 120.2(4) . . ?
C23 C22 C21 119.4(4) . . ?
C22 C23 C18 120.6(4) . . ?
C25 C24 C29 118.4(4) . . ?
C25 C24 C16 121.4(4) . . ?
C29 C24 C16 120.2(4) . . ?
C26 C25 C24 120.8(4) . . ?
C27 C26 C25 119.7(4) . . ?
C26 C27 C28 120.6(4) . . ?
C29 C28 C27 119.7(4) . . ?
C28 C29 C24 120.7(4) . . ?
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 1.939(2) . ?
W1 F2 1.982(2) . ?
W1 C17 2.024(4) . ?
W1 C16 2.049(4) . ?
W1 N5 2.155(3) . ?
W1 N3 2.175(3) . ?
W1 N1 2.252(3) . ?
N1 C2 1.351(5) . ?
N1 N2 1.373(4) . ?
N2 C4 1.347(5) . ?
N2 B1 1.547(6) . ?
C1 C2 1.493(6) . ?
C2 C3 1.391(6) . ?
C3 C4 1.377(6) . ?
C4 C5 1.499(5) . ?
N3 C7 1.340(5) . ?
N3 N4 1.384(4) . ?
N4 C9 1.354(5) . ?
N4 B1 1.543(6) . ?
C6 C7 1.501(5) . ?
C7 C8 1.389(6) . ?
C8 C9 1.379(6) . ?
C9 C10 1.491(5) . ?
N5 C12 1.351(5) . ?
N5 N6 1.374(4) . ?
N6 C14 1.354(5) . ?
N6 B1 1.533(6) . ?
C11 C12 1.491(6) . ?
C12 C13 1.383(6) . ?
C13 C14 1.375(6) . ?
C14 C15 1.497(6) . ?
C16 C17 1.319(5) . ?
C16 C24 1.462(5) . ?
C17 C18 1.465(5) . ?
C18 C19 1.395(6) . ?
C18 C23 1.401(6) . ?
C19 C20 1.378(6) . ?
C20 C21 1.374(6) . ?
C21 C22 1.393(6) . ?
C22 C23 1.386(6) . ?
C24 C25 1.393(5) . ?
C24 C29 1.396(6) . ?
C25 C26 1.389(6) . ?
C26 C27 1.365(7) . ?
C27 C28 1.390(7) . ?
C28 C29 1.377(6) . ?
