#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:40:51 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179802 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/98/7009894.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_7009894
loop_
_publ_author_name
'Wadepohl, Hubert'
'Arnold, Ulrich'
'Kohl, Ute'
'Pritzkow, Hans'
'Wolf, Andreas'
_publ_section_title
;
 Hydroboration of metal--carbon triple bonds †
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3554
_journal_paper_doi               10.1039/b004256k
_journal_year                    2000
_chemical_formula_sum            'C31 H47 B O4 W'
_chemical_formula_weight         678.35
_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                103.00(13)
_cell_angle_beta                 97.29(13)
_cell_angle_gamma                97.15(13)
_cell_formula_units_Z            2
_cell_length_a                   8.829(14)
_cell_length_b                   12.33(2)
_cell_length_c                   14.24(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11.6
_cell_volume                     1479(4)
_computing_cell_refinement       'DIF4 (Stoe)'
_computing_data_collection       'DIF4 (Stoe)'
_computing_data_reduction        'REDU4 (Stoe)'
_computing_molecular_graphics    'ORTEP (C.K.Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      218(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens-Stoe AED2'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6129
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.936
_exptl_absorpt_correction_T_max  0.3162
_exptl_absorpt_correction_T_min  0.1563
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         6129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0494P)²+1.2283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                5762
_reflns_number_total             6129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004256k.txt
_cod_data_source_block           complex14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.2283P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.2283P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1480(4)
_cod_database_code               7009894
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.396528(15) 0.264287(11) 0.721406(9) 0.02412(6) Uani 1 d . . .
O1 O 0.6772(4) 0.1745(3) 0.6354(3) 0.0525(9) Uani 1 d . . .
O2 O 0.4024(4) 0.2629(3) 0.9369(2) 0.0399(7) Uani 1 d . . .
O3 O 0.9027(4) 0.7745(3) 0.7489(3) 0.0435(7) Uani 1 d . . .
O4 O 0.9289(3) 0.5834(2) 0.7501(2) 0.0350(6) Uani 1 d . . .
B1 B 0.9678(5) 0.6803(4) 0.7219(3) 0.0354(10) Uani 1 d . . .
C1 C 0.5769(5) 0.2091(3) 0.6718(3) 0.0350(8) Uani 1 d . . .
C2 C 0.4660(4) 0.2317(3) 0.8668(3) 0.0295(8) Uani 1 d . . .
C3 C 0.6034(5) 0.1682(4) 0.8825(3) 0.0423(10) Uani 1 d . . .
H3A H 0.5816 0.0947 0.8353 0.048(5) Uiso 1 calc R . .
H3B H 0.6957 0.2106 0.8685 0.048(5) Uiso 1 calc R . .
C4 C 0.6394(8) 0.1493(6) 0.9848(4) 0.0714(18) Uani 1 d . . .
H4A H 0.7308 0.1133 0.9895 0.066(4) Uiso 1 calc R . .
H4B H 0.5524 0.1013 0.9974 0.066(4) Uiso 1 calc R . .
H4C H 0.6578 0.2212 1.0326 0.066(4) Uiso 1 calc R . .
C5 C 0.5865(4) 0.4122(3) 0.8116(3) 0.0290(7) Uani 1 d . . .
H5 H 0.6100 0.3652 0.8532 0.114(16) Uiso 1 calc R . .
C6 C 0.4371(4) 0.4471(3) 0.8046(3) 0.0292(8) Uani 1 d . . .
C7 C 0.3722(4) 0.4389(3) 0.7066(3) 0.0326(8) Uani 1 d . . .
H7 H 0.2742 0.4584 0.6907 0.114(16) Uiso 1 calc R . .
C8 C 0.4615(5) 0.3998(3) 0.6331(3) 0.0340(8) Uani 1 d . . .
H8 H 0.4121 0.3502 0.5739 0.114(16) Uiso 1 calc R . .
C9 C 0.6308(5) 0.4359(3) 0.6483(3) 0.0319(8) Uani 1 d . . .
C10 C 0.7079(4) 0.4497(3) 0.7533(3) 0.0287(7) Uani 1 d . . .
H10 H 0.7820 0.3955 0.7508 0.030(11) Uiso 1 calc R . .
C11 C 0.8030(4) 0.5680(3) 0.8052(3) 0.0312(8) Uani 1 d . . .
C12 C 0.7043(5) 0.6609(3) 0.8046(3) 0.0341(8) Uani 1 d . . .
H12A H 0.6431 0.6631 0.8576 0.048(5) Uiso 1 calc R . .
H12B H 0.6315 0.6400 0.7431 0.048(5) Uiso 1 calc R . .
C13 C 0.7901(5) 0.7800(4) 0.8156(3) 0.0385(9) Uani 1 d . . .
C14 C 0.3601(5) 0.4963(4) 0.8897(3) 0.0404(10) Uani 1 d . . .
H14A H 0.4079 0.5740 0.9181 0.052(8) Uiso 1 calc R . .
H14B H 0.3721 0.4531 0.9385 0.052(8) Uiso 1 calc R . .
H14C H 0.2510 0.4935 0.8672 0.052(8) Uiso 1 calc R . .
C15 C 0.7047(6) 0.4468(4) 0.5738(3) 0.0423(10) Uani 1 d . . .
C16 C 0.8787(5) 0.5655(4) 0.9078(3) 0.0411(10) Uani 1 d . . .
H16A H 0.9117 0.4930 0.9057 0.066(4) Uiso 1 calc R . .
H16B H 0.8046 0.5772 0.9524 0.066(4) Uiso 1 calc R . .
H16C H 0.9677 0.6248 0.9300 0.066(4) Uiso 1 calc R . .
C17 C 0.6786(6) 0.8536(4) 0.7834(4) 0.0529(12) Uani 1 d . . .
H17A H 0.6009 0.8610 0.8259 0.066(4) Uiso 1 calc R . .
H17B H 0.6286 0.8193 0.7167 0.066(4) Uiso 1 calc R . .
H17C H 0.7348 0.9275 0.7868 0.066(4) Uiso 1 calc R . .
C18 C 0.8761(8) 0.8370(5) 0.9175(4) 0.0636(15) Uani 1 d . . .
H18A H 0.8061 0.8345 0.9646 0.066(4) Uiso 1 calc R . .
H18B H 0.9158 0.9148 0.9204 0.066(4) Uiso 1 calc R . .
H18C H 0.9614 0.7980 0.9327 0.066(4) Uiso 1 calc R . .
C19 C 1.1017(5) 0.6829(5) 0.6583(3) 0.0456(11) Uani 1 d . . .
H19A H 1.0932 0.6088 0.6132 0.048(5) Uiso 1 calc R . .
H19B H 1.0890 0.7382 0.6193 0.048(5) Uiso 1 calc R . .
C20 C 1.2618(6) 0.7130(4) 0.7204(4) 0.0509(12) Uani 1 d . . .
H20A H 1.3399 0.7135 0.6782 0.066(4) Uiso 1 calc R . .
H20B H 1.2759 0.6575 0.7581 0.066(4) Uiso 1 calc R . .
H20C H 1.2716 0.7869 0.7643 0.066(4) Uiso 1 calc R . .
C21 C 0.2308(5) 0.1510(3) 0.5869(3) 0.0315(8) Uani 1 d . . .
C22 C 0.2786(4) 0.0766(3) 0.6451(3) 0.0291(8) Uani 1 d . . .
C23 C 0.2198(4) 0.1047(3) 0.7350(3) 0.0288(7) Uani 1 d . . .
C24 C 0.1378(4) 0.1978(3) 0.7340(3) 0.0317(8) Uani 1 d . . .
C25 C 0.1415(4) 0.2244(3) 0.6416(3) 0.0301(8) Uani 1 d . . .
C26 C 0.2475(5) 0.1389(4) 0.4811(3) 0.0358(9) Uani 1 d . . .
H26A H 0.3482 0.1168 0.4709 0.048(5) Uiso 1 calc R . .
H26B H 0.2442 0.2117 0.4648 0.048(5) Uiso 1 calc R . .
C27 C 0.1195(6) 0.0509(4) 0.4135(3) 0.0446(11) Uani 1 d . . .
H27A H 0.1315 0.0471 0.3461 0.066(4) Uiso 1 calc R . .
H27B H 0.0196 0.0718 0.4243 0.066(4) Uiso 1 calc R . .
H27C H 0.1260 -0.0221 0.4272 0.066(4) Uiso 1 calc R . .
C28 C 0.3571(5) -0.0225(3) 0.6135(3) 0.0397(9) Uani 1 d . . .
H28A H 0.2808 -0.0904 0.5925 0.053(4) Uiso 1 calc R . .
H28B H 0.4313 -0.0288 0.6676 0.053(4) Uiso 1 calc R . .
H28C H 0.4104 -0.0128 0.5597 0.053(4) Uiso 1 calc R . .
C29 C 0.2171(6) 0.0348(4) 0.8082(3) 0.0408(10) Uani 1 d . . .
H29A H 0.1293 -0.0255 0.7874 0.053(4) Uiso 1 calc R . .
H29B H 0.2083 0.0817 0.8712 0.053(4) Uiso 1 calc R . .
H29C H 0.3119 0.0029 0.8135 0.053(4) Uiso 1 calc R . .
C30 C 0.0454(5) 0.2448(4) 0.8102(3) 0.0449(11) Uani 1 d . . .
H30A H 0.1045 0.2541 0.8745 0.053(4) Uiso 1 calc R . .
H30B H -0.0503 0.1935 0.8031 0.053(4) Uiso 1 calc R . .
H30C H 0.0222 0.3174 0.8022 0.053(4) Uiso 1 calc R . .
C31 C 0.0439(5) 0.3012(4) 0.6015(3) 0.0399(9) Uani 1 d . . .
H31A H -0.0535 0.2576 0.5654 0.053(4) Uiso 1 calc R . .
H31B H 0.0986 0.3363 0.5583 0.053(4) Uiso 1 calc R . .
H31C H 0.0240 0.3591 0.6550 0.053(4) Uiso 1 calc R . .
H15A H 0.814(6) 0.468(4) 0.580(3) 0.034(11) Uiso 1 d . . .
H15B H 0.640(5) 0.435(4) 0.514(3) 0.028(11) Uiso 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'
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
C1 W1 C2 92.5(2) . . ?
C1 W1 C7 113.7(2) . . ?
C2 W1 C7 120.86(18) . . ?
C1 W1 C6 115.2(2) . . ?
C2 W1 C6 84.5(2) . . ?
C7 W1 C6 36.66(16) . . ?
C1 W1 C21 91.7(2) . . ?
C2 W1 C21 129.40(18) . . ?
C7 W1 C21 103.0(2) . . ?
C6 W1 C21 137.03(17) . . ?
C1 W1 C25 127.30(19) . . ?
C2 W1 C25 122.81(17) . . ?
C7 W1 C25 82.4(2) . . ?
C6 W1 C25 106.7(2) . . ?
C21 W1 C25 36.08(16) . . ?
C1 W1 C5 81.5(2) . . ?
C2 W1 C5 71.69(19) . . ?
C7 W1 C5 62.17(18) . . ?
C6 W1 C5 36.42(16) . . ?
C21 W1 C5 158.36(15) . . ?
C25 W1 C5 142.43(17) . . ?
C1 W1 C8 80.5(2) . . ?
C2 W1 C8 139.00(17) . . ?
C7 W1 C8 35.87(16) . . ?
C6 W1 C8 63.19(18) . . ?
C21 W1 C8 91.36(19) . . ?
C25 W1 C8 91.79(19) . . ?
C5 W1 C8 67.33(18) . . ?
C1 W1 C22 82.0(2) . . ?
C2 W1 C22 95.4(2) . . ?
C7 W1 C22 138.12(17) . . ?
C6 W1 C22 162.80(15) . . ?
C21 W1 C22 35.69(16) . . ?
C25 W1 C22 59.08(19) . . ?
C5 W1 C22 158.45(15) . . ?
C8 W1 C22 123.02(18) . . ?
C1 W1 C24 140.41(18) . . ?
C2 W1 C24 87.46(19) . . ?
C7 W1 C24 99.79(19) . . ?
C6 W1 C24 104.2(2) . . ?
C21 W1 C24 59.54(19) . . ?
C25 W1 C24 35.38(15) . . ?
C5 W1 C24 135.01(17) . . ?
C8 W1 C24 122.96(18) . . ?
C22 W1 C24 58.66(18) . . ?
C1 W1 C23 108.3(2) . . ?
C2 W1 C23 72.25(19) . . ?
C7 W1 C23 134.57(17) . . ?
C6 W1 C23 131.14(17) . . ?
C21 W1 C23 58.67(18) . . ?
C25 W1 C23 58.21(18) . . ?
C5 W1 C23 142.96(15) . . ?
C8 W1 C23 148.26(15) . . ?
C22 W1 C23 34.76(15) . . ?
C24 W1 C23 34.83(15) . . ?
B1 O3 C13 121.3(4) . . ?
B1 O4 C11 122.6(3) . . ?
O3 B1 O4 123.7(4) . . ?
O3 B1 C19 119.3(4) . . ?
O4 B1 C19 117.0(4) . . ?
O1 C1 W1 174.9(4) . . ?
O2 C2 C3 117.0(4) . . ?
O2 C2 W1 123.4(3) . . ?
C3 C2 W1 119.6(3) . . ?
C4 C3 C2 115.0(4) . . ?
C6 C5 C10 121.6(3) . . ?
C6 C5 W1 69.1(2) . . ?
C10 C5 W1 113.9(3) . . ?
C7 C6 C5 111.9(4) . . ?
C7 C6 C14 122.3(4) . . ?
C5 C6 C14 125.6(4) . . ?
C7 C6 W1 71.1(3) . . ?
C5 C6 W1 74.5(3) . . ?
C14 C6 W1 125.8(3) . . ?
C6 C7 C8 117.2(4) . . ?
C6 C7 W1 72.3(3) . . ?
C8 C7 W1 76.7(3) . . ?
C7 C8 C9 121.1(4) . . ?
C7 C8 W1 67.4(2) . . ?
C9 C8 W1 111.0(3) . . ?
C15 C9 C8 121.3(4) . . ?
C15 C9 C10 125.4(4) . . ?
C8 C9 C10 113.2(3) . . ?
C9 C10 C5 108.8(3) . . ?
C9 C10 C11 116.0(3) . . ?
C5 C10 C11 112.3(3) . . ?
O4 C11 C12 110.1(3) . . ?
O4 C11 C16 106.3(3) . . ?
C12 C11 C16 113.8(4) . . ?
O4 C11 C10 105.7(3) . . ?
C12 C11 C10 111.4(3) . . ?
C16 C11 C10 109.2(4) . . ?
C11 C12 C13 116.8(4) . . ?
O3 C13 C17 105.7(4) . . ?
O3 C13 C18 107.6(4) . . ?
C17 C13 C18 109.7(4) . . ?
O3 C13 C12 108.7(4) . . ?
C17 C13 C12 110.0(4) . . ?
C18 C13 C12 114.7(4) . . ?
C20 C19 B1 112.5(4) . . ?
C22 C21 C25 107.5(4) . . ?
C22 C21 C26 125.1(4) . . ?
C25 C21 C26 126.6(4) . . ?
C22 C21 W1 74.3(2) . . ?
C25 C21 W1 72.7(2) . . ?
C26 C21 W1 127.0(3) . . ?
C23 C22 C21 108.0(4) . . ?
C23 C22 C28 125.1(4) . . ?
C21 C22 C28 126.4(4) . . ?
C23 C22 W1 74.5(2) . . ?
C21 C22 W1 70.0(2) . . ?
C28 C22 W1 127.4(3) . . ?
C22 C23 C24 108.4(4) . . ?
C22 C23 C29 125.3(4) . . ?
C24 C23 C29 125.3(4) . . ?
C22 C23 W1 70.8(3) . . ?
C24 C23 W1 71.0(2) . . ?
C29 C23 W1 133.2(3) . . ?
C25 C24 C23 107.5(4) . . ?
C25 C24 C30 126.8(4) . . ?
C23 C24 C30 125.0(4) . . ?
C25 C24 W1 70.7(2) . . ?
C23 C24 W1 74.2(3) . . ?
C30 C24 W1 127.8(3) . . ?
C24 C25 C21 108.5(4) . . ?
C24 C25 C31 125.2(4) . . ?
C21 C25 C31 125.4(4) . . ?
C24 C25 W1 73.9(2) . . ?
C21 C25 W1 71.2(2) . . ?
C31 C25 W1 129.2(3) . . ?
C21 C26 C27 111.6(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 C1 1.959(5) . ?
W1 C2 2.222(5) . ?
W1 C7 2.244(5) . ?
W1 C6 2.260(6) . ?
W1 C21 2.311(6) . ?
W1 C25 2.329(6) . ?
W1 C5 2.330(6) . ?
W1 C8 2.365(5) . ?
W1 C22 2.367(6) . ?
W1 C24 2.372(5) . ?
W1 C23 2.415(6) . ?
O1 C1 1.160(5) . ?
O2 C2 1.218(5) . ?
O3 B1 1.359(6) . ?
O3 C13 1.457(6) . ?
O4 B1 1.363(6) . ?
O4 C11 1.457(5) . ?
B1 C19 1.579(7) . ?
C2 C3 1.543(6) . ?
C3 C4 1.527(7) . ?
C5 C6 1.436(6) . ?
C5 C10 1.526(6) . ?
C6 C7 1.417(6) . ?
C6 C14 1.509(6) . ?
C7 C8 1.424(6) . ?
C8 C9 1.479(6) . ?
C9 C15 1.336(6) . ?
C9 C10 1.525(6) . ?
C10 C11 1.560(6) . ?
C11 C12 1.525(6) . ?
C11 C16 1.536(6) . ?
C12 C13 1.531(6) . ?
C13 C17 1.516(7) . ?
C13 C18 1.518(7) . ?
C19 C20 1.524(7) . ?
C21 C22 1.434(6) . ?
C21 C25 1.437(6) . ?
C21 C26 1.508(6) . ?
C22 C23 1.429(6) . ?
C22 C28 1.490(6) . ?
C23 C24 1.433(6) . ?
C23 C29 1.494(6) . ?
C24 C25 1.429(6) . ?
C24 C30 1.495(7) . ?
C25 C31 1.514(6) . ?
C26 C27 1.526(7) . ?
