#------------------------------------------------------------------------------
#$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100871.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_1100871
loop_
_publ_author_name
'Jamison, Gregory M.'
'Wheeler, David R.'
'Loy, Douglas A.'
'Ziller, Joseph W.'
_publ_section_title
;
 Double Phosphaalkyne Insertion to a Tungsten Alkylidene: 
 Formation of a Diphosphametallabicyclobutane
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2245
_journal_page_last               2247
_journal_paper_doi               10.1021/om050150o
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C35 H51 F12 N O2 P2 W'
_chemical_formula_weight         991.56
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 117.670(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.110(5)
_cell_length_b                   10.6323(9)
_cell_length_c                   20.577(2)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    163
_cell_measurement_theta_max      11.70
_cell_measurement_theta_min      5.10
_cell_volume                     8159.4(14)
_diffrn_ambient_temperature      163
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5419
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 99
_diffrn_standards_interval_time  ?
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.996
_exptl_absorpt_correction_T_max  0.6052
_exptl_absorpt_correction_T_min  0.4794
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment    ?
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_obs          0.0317
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0229P)²+57.0484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0714
_refine_ls_wR_factor_obs         0.0650
_reflns_number_observed          4385
_reflns_number_total             5334
_reflns_observed_criterion       >2sigma(I)
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+57.0484P] 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^)+(0.0229P)^2^+57.0484P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1100871
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'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
W1 W 0.626961(6) 0.39317(2) -0.225787(12) 0.01704(9) Uani 1 d . .
P1 P 0.57991(4) 0.2435(2) -0.23887(9) 0.0237(4) Uani 1 d . .
P2 P 0.60800(4) 0.2972(2) -0.12310(8) 0.0245(4) Uani 1 d . .
N1 N 0.63148(12) 0.3427(5) -0.3007(3) 0.0228(12) Uani 1 d . .
O1 O 0.67039(11) 0.4656(4) -0.1530(2) 0.0336(11) Uani 1 d . .
O2 O 0.59600(10) 0.5366(4) -0.2549(2) 0.0206(9) Uani 1 d . .
C1 C 0.6278(2) 0.2171(6) -0.1770(3) 0.0221(14) Uani 1 d . .
C2 C 0.6501(2) 0.0997(6) -0.1668(3) 0.0269(14) Uani 1 d . .
C3 C 0.6407(2) 0.0437(6) -0.2425(3) 0.031(2) Uani 1 d . .
H3A H 0.6551(2) -0.0322(6) -0.2362(3) 0.047 Uiso 1 calc R .
H3B H 0.6460(2) 0.1056(6) -0.2715(3) 0.047 Uiso 1 calc R .
H3C H 0.6152(2) 0.0221(6) -0.2680(3) 0.047 Uiso 1 calc R .
C4 C 0.6899(2) 0.1316(6) -0.1274(3) 0.034(2) Uani 1 d . .
H4A H 0.7039(2) 0.0550(6) -0.1212(3) 0.051 Uiso 1 calc R .
H4B H 0.6960(2) 0.1676(6) -0.0792(3) 0.051 Uiso 1 calc R .
H4C H 0.6953(2) 0.1928(6) -0.1565(3) 0.051 Uiso 1 calc R .
C5 C 0.6421(2) 0.0007(6) -0.1227(4) 0.037(2) Uani 1 d . .
H5A H 0.6568(2) -0.0742(6) -0.1168(4) 0.056 Uiso 1 calc R .
H5B H 0.6167(2) -0.0222(6) -0.1486(4) 0.056 Uiso 1 calc R .
H5C H 0.6477(2) 0.0348(6) -0.0743(4) 0.056 Uiso 1 calc R .
C6 C 0.5946(2) 0.1970(6) -0.0655(3) 0.027(2) Uani 1 d . .
C7 C 0.6156(2) 0.1960(6) 0.0057(3) 0.030(2) Uani 1 d . .
H7A H 0.6060(2) 0.1465(6) 0.0309(3) 0.036 Uiso 1 calc R .
C8 C 0.6512(2) 0.2542(7) 0.0574(3) 0.033(2) Uani 1 d . .
C9 C 0.6654(2) 0.1845(11) 0.1305(4) 0.085(3) Uani 1 d . .
H9A H 0.6473(2) 0.1865(11) 0.1478(4) 0.127 Uiso 1 calc R .
H9B H 0.6874(2) 0.2253(11) 0.1667(4) 0.127 Uiso 1 calc R .
H9C H 0.6706(2) 0.0970(11) 0.1238(4) 0.127 Uiso 1 calc R .
C10 C 0.6799(2) 0.2484(9) 0.0334(4) 0.064(3) Uani 1 d . .
H10A H 0.7018(2) 0.2885(9) 0.0705(4) 0.096 Uiso 1 calc R .
H10B H 0.6717(2) 0.2926(9) -0.0135(4) 0.096 Uiso 1 calc R .
H10C H 0.6849(2) 0.1603(9) 0.0274(4) 0.096 Uiso 1 calc R .
C11 C 0.6441(2) 0.3898(8) 0.0691(5) 0.074(3) Uani 1 d . .
H11A H 0.6254(2) 0.3931(8) 0.0847(5) 0.111 Uiso 1 calc R .
H11B H 0.6361(2) 0.4365(8) 0.0231(5) 0.111 Uiso 1 calc R .
H11C H 0.6662(2) 0.4277(8) 0.1070(5) 0.111 Uiso 1 calc R .
C12 C 0.5557(2) 0.1419(6) -0.0983(3) 0.0249(15) Uani 1 d . .
C13 C 0.5463(2) 0.0919(7) -0.0393(3) 0.037(2) Uani 1 d . .
H13A H 0.5629(2) 0.0244(7) -0.0116(3) 0.055 Uiso 1 calc R .
H13B H 0.5217(2) 0.0590(7) -0.0629(3) 0.055 Uiso 1 calc R .
H13C H 0.5481(2) 0.1603(7) -0.0058(3) 0.055 Uiso 1 calc R .
C14 C 0.5503(2) 0.0313(6) -0.1505(3) 0.035(2) Uani 1 d . .
H14A H 0.5678(2) -0.0350(6) -0.1241(3) 0.052 Uiso 1 calc R .
H14B H 0.5538(2) 0.0604(6) -0.1919(3) 0.052 Uiso 1 calc R .
H14C H 0.5260(2) -0.0022(6) -0.1687(3) 0.052 Uiso 1 calc R .
C15 C 0.5286(2) 0.2461(6) -0.1387(3) 0.033(2) Uani 1 d . .
H15A H 0.5335(2) 0.2813(6) -0.1772(3) 0.049 Uiso 1 calc R .
H15B H 0.5307(2) 0.3125(6) -0.1039(3) 0.049 Uiso 1 calc R .
H15C H 0.5043(2) 0.2112(6) -0.1610(3) 0.049 Uiso 1 calc R .
C16 C 0.6338(2) 0.3034(5) -0.3643(3) 0.0201(14) Uani 1 d . .
C17 C 0.6667(2) 0.2655(6) -0.3585(3) 0.0234(15) Uani 1 d . .
C18 C 0.6670(2) 0.2162(6) -0.4209(3) 0.030(2) Uani 1 d . .
H18A H 0.6890(2) 0.1894(6) -0.4186(3) 0.035 Uiso 1 calc R .
C19 C 0.6356(2) 0.2055(6) -0.4863(3) 0.033(2) Uani 1 d . .
H19A H 0.6360(2) 0.1692(6) -0.5280(3) 0.040 Uiso 1 calc R .
C20 C 0.6041(2) 0.2473(6) -0.4905(3) 0.032(2) Uani 1 d . .
H20A H 0.5830(2) 0.2416(6) -0.5362(3) 0.038 Uiso 1 calc R .
C21 C 0.6016(2) 0.2977(6) -0.4310(3) 0.0231(14) Uani 1 d . .
C22 C 0.7020(2) 0.2794(6) -0.2885(3) 0.027(2) Uani 1 d . .
H22A H 0.6962(2) 0.3068(6) -0.2487(3) 0.032 Uiso 1 calc R .
C23 C 0.7223(2) 0.1558(6) -0.2646(4) 0.037(2) Uani 1 d . .
H23A H 0.7068(2) 0.0918(6) -0.2596(4) 0.056 Uiso 1 calc R .
H23B H 0.7437(2) 0.1673(6) -0.2173(4) 0.056 Uiso 1 calc R .
H23C H 0.7294(2) 0.1285(6) -0.3015(4) 0.056 Uiso 1 calc R .
C24 C 0.7252(2) 0.3800(6) -0.2967(4) 0.039(2) Uani 1 d . .
H24A H 0.7117(2) 0.4589(6) -0.3121(4) 0.059 Uiso 1 calc R .
H24B H 0.7323(2) 0.3539(6) -0.3337(4) 0.059 Uiso 1 calc R .
H24C H 0.7466(2) 0.3926(6) -0.2495(4) 0.059 Uiso 1 calc R .
C25 C 0.5664(2) 0.3454(7) -0.4389(3) 0.032(2) Uani 1 d . .
H25A H 0.5713(2) 0.3932(7) -0.3933(3) 0.038 Uiso 1 calc R .
C26 C 0.5414(2) 0.2363(8) -0.4455(4) 0.054(2) Uani 1 d . .
H26A H 0.5186(2) 0.2696(8) -0.4506(4) 0.082 Uiso 1 calc R .
H26B H 0.5526(2) 0.1837(8) -0.4014(4) 0.082 Uiso 1 calc R .
H26C H 0.5369(2) 0.1856(8) -0.4888(4) 0.082 Uiso 1 calc R .
C27 C 0.5480(2) 0.4349(8) -0.5040(4) 0.054(2) Uani 1 d . .
H27A H 0.5252(2) 0.4636(8) -0.5070(4) 0.081 Uiso 1 calc R .
H27B H 0.5434(2) 0.3911(8) -0.5494(4) 0.081 Uiso 1 calc R .
H27C H 0.5635(2) 0.5076(8) -0.4972(4) 0.081 Uiso 1 calc R .
C28 C 0.6956(2) 0.5498(6) -0.1080(3) 0.028(2) Uani 1 d . .
C29 C 0.7320(2) 0.4828(7) -0.0729(4) 0.042(2) Uani 1 d . .
C30 C 0.6958(2) 0.6589(7) -0.1562(4) 0.045(2) Uani 1 d . .
C31 C 0.6869(2) 0.5998(9) -0.0489(4) 0.063(2) Uani 1 d . .
H31A H 0.6868(2) 0.5300(9) -0.0178(4) 0.094 Uiso 1 calc R .
H31B H 0.6632(2) 0.6397(9) -0.0720(4) 0.094 Uiso 1 calc R .
H31C H 0.7050(2) 0.6617(9) -0.0188(4) 0.094 Uiso 1 calc R .
C32 C 0.56384(15) 0.5989(6) -0.2732(3) 0.0228(14) Uani 1 d . .
C33 C 0.5608(2) 0.7018(7) -0.3287(4) 0.040(2) Uani 1 d . .
C34 C 0.5667(2) 0.6590(7) -0.2030(4) 0.032(2) Uani 1 d . .
C35 C 0.5310(2) 0.5152(6) -0.3071(4) 0.036(2) Uani 1 d . .
H35A H 0.5292(2) 0.4767(6) -0.3520(4) 0.054 Uiso 1 calc R .
H35B H 0.5095(2) 0.5656(6) -0.3190(4) 0.054 Uiso 1 calc R .
H35C H 0.5331(2) 0.4490(6) -0.2721(4) 0.054 Uiso 1 calc R .
F1 F 0.73995(11) 0.4316(5) -0.1221(2) 0.0626(13) Uani 1 d . .
F2 F 0.75844(11) 0.5604(4) -0.0321(3) 0.0670(14) Uani 1 d . .
F3 F 0.73181(11) 0.3914(5) -0.0294(2) 0.0633(13) Uani 1 d . .
F4 F 0.71911(14) 0.7472(5) -0.1180(4) 0.106(2) Uani 1 d . .
F5 F 0.66368(11) 0.7128(4) -0.1892(2) 0.0527(12) Uani 1 d . .
F6 F 0.7035(2) 0.6214(6) -0.2079(3) 0.096(2) Uani 1 d . .
F7 F 0.55970(14) 0.6502(4) -0.3878(2) 0.0647(14) Uani 1 d . .
F8 F 0.58844(12) 0.7803(4) -0.3018(3) 0.0620(13) Uani 1 d . .
F9 F 0.53139(12) 0.7710(4) -0.3498(2) 0.0608(13) Uani 1 d . .
F10 F 0.53921(11) 0.7328(4) -0.2148(2) 0.0533(12) Uani 1 d . .
F11 F 0.56757(13) 0.5711(4) -0.1565(2) 0.0589(13) Uani 1 d . .
F12 F 0.59603(11) 0.7281(4) -0.1676(2) 0.0558(12) Uani 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'
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'
P P 0.1023 0.0942 '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'
