#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:55:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178630 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/41/4074141.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_4074141
loop_
_publ_author_name
'Lis, Jr., Edward C.'
'Delafuente, David A.'
'Lin, Yunqing'
'Mocella, Christopher J.'
'Todd, Michael A.'
'Liu, Weijun'
'Sabat, Michal'
'Myers, William H.'
'Harman, W. Dean'
_publ_section_title
;
 The Uncommon Reactivity of Dihapto-Coordinated Nitrile, Ketone, and
 Alkene Ligands When Bound to a Powerful π-Base
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5051
_journal_page_last               5058
_journal_paper_doi               10.1021/om060434o
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C18 H25 B F3 Mo N9 O5 S'
_chemical_formula_weight         643.28
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.8310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9609(4)
_cell_length_b                   13.6846(7)
_cell_length_c                   24.5781(13)
_cell_measurement_reflns_used    9454
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.381
_cell_measurement_theta_min      3.033
_cell_volume                     2671.6(2)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            31696
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.801926
_exptl_absorpt_correction_T_min  0.672148
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            olive-green
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         9139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0447
_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)+(0.0541P)²+1.4124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                7208
_reflns_number_total             9139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060434osi20060518_120441.cif
_cod_data_source_block           c18h25bf3mon9o5s
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4074141
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Mo Mo 0.14458(2) 0.495222(11) 0.163210(7) 0.01799(6) Uani 1 1 d
S S 0.71310(8) 0.39206(5) 0.38080(3) 0.03522(14) Uani 1 1 d
F1 F 0.6122(3) 0.50174(19) 0.45892(14) 0.1023(11) Uani 1 1 d
F2 F 0.8298(3) 0.55641(14) 0.42319(10) 0.0803(7) Uani 1 1 d
F3 F 0.8537(3) 0.43587(16) 0.47667(7) 0.0639(6) Uani 1 1 d
O1 O 0.3753(2) 0.49945(10) 0.21196(7) 0.0271(3) Uani 1 1 d
O2 O -0.0651(3) 0.64403(17) 0.21281(10) 0.0612(7) Uani 1 1 d
O3 O 0.6484(3) 0.30815(15) 0.40736(11) 0.0583(6) Uani 1 1 d
O4 O 0.5942(4) 0.4435(3) 0.34621(12) 0.0915(10) Uani 1 1 d
O5 O 0.8748(3) 0.37837(18) 0.36051(8) 0.0506(5) Uani 1 1 d
N1 N -0.0273(2) 0.37711(14) 0.18189(8) 0.0251(4) Uani 1 1 d
N2 N -0.0589(2) 0.30215(14) 0.14609(8) 0.0276(4) Uani 1 1 d
N3 N -0.0379(2) 0.49200(12) 0.09303(7) 0.0217(3) Uani 1 1 d
N4 N -0.0733(2) 0.40786(13) 0.06520(7) 0.0232(3) Uani 1 1 d
N5 N 0.2798(2) 0.37971(13) 0.11789(7) 0.0225(3) Uani 1 1 d
N6 N 0.1884(2) 0.31133(13) 0.08819(8) 0.0265(4) Uani 1 1 d
N7 N 0.2734(2) 0.60965(13) 0.12014(7) 0.0223(3) Uani 1 1 d
N8 N 0.3127(2) 0.75468(13) 0.08482(8) 0.0277(4) Uani 1 1 d
N9 N 0.0239(2) 0.58420(15) 0.19427(8) 0.0297(4) Uani 1 1 d
C2 C 0.2567(3) 0.44600(17) 0.24188(9) 0.0267(4) Uani 1 1 d
C3 C 0.2074(4) 0.4953(3) 0.29315(11) 0.0448(7) Uani 1 1 d
C4 C 0.3100(4) 0.3416(2) 0.24956(12) 0.0389(6) Uani 1 1 d
C5 C 0.4651(4) 0.5839(2) 0.23541(12) 0.0390(6) Uani 1 1 d
C6 C -0.1690(3) 0.2400(2) 0.16743(13) 0.0391(6) Uani 1 1 d
C7 C -0.2094(3) 0.2744(2) 0.21689(13) 0.0451(7) Uani 1 1 d
C8 C -0.1184(3) 0.3606(2) 0.22447(11) 0.0367(6) Uani 1 1 d
C9 C -0.1866(3) 0.42647(19) 0.02322(9) 0.0283(4) Uani 1 1 d
C10 C -0.2259(3) 0.52393(19) 0.02342(10) 0.0297(5) Uani 1 1 d
C11 C -0.1305(3) 0.56225(17) 0.06782(9) 0.0249(4) Uani 1 1 d
C12 C 0.2934(3) 0.24989(18) 0.06479(11) 0.0367(6) Uani 1 1 d
C13 C 0.4557(3) 0.2770(2) 0.07902(12) 0.0386(6) Uani 1 1 d
C14 C 0.4422(3) 0.35827(17) 0.11232(10) 0.0285(4) Uani 1 1 d
C15 C 0.2091(3) 0.69866(16) 0.11191(9) 0.0249(4) Uani 1 1 d
C16 C 0.4528(3) 0.70047(17) 0.07588(10) 0.0291(5) Uani 1 1 d
C17 C 0.4276(3) 0.61138(17) 0.09745(9) 0.0258(4) Uani 1 1 d
C18 C 0.2778(4) 0.85576(19) 0.06741(15) 0.0405(6) Uani 1 1 d
C19 C 0.7532(4) 0.4758(2) 0.43738(13) 0.0439(6) Uani 1 1 d
B B -0.0040(3) 0.30945(18) 0.08760(11) 0.0273(5) Uani 1 1 d
H1B H -0.052(3) 0.2557(18) 0.0610(10) 0.024(6) Uiso 1 1 d
H3A H 0.127(5) 0.449(3) 0.3061(15) 0.069(12) Uiso 1 1 d
H3B H 0.168(4) 0.565(3) 0.2889(13) 0.046(9) Uiso 1 1 d
H3C H 0.301(4) 0.4933(19) 0.3235(14) 0.036(8) Uiso 1 1 d
H4A H 0.341(4) 0.312(2) 0.2146(13) 0.039(8) Uiso 1 1 d
H4B H 0.226(4) 0.311(3) 0.2609(14) 0.054(10) Uiso 1 1 d
H4C H 0.409(4) 0.336(2) 0.2779(14) 0.052(9) Uiso 1 1 d
H5A H 0.370(4) 0.633(3) 0.2473(14) 0.056(10) Uiso 1 1 d
H5B H 0.542(4) 0.605(2) 0.2080(12) 0.036(8) Uiso 1 1 d
H5C H 0.540(4) 0.562(2) 0.2648(14) 0.052(9) Uiso 1 1 d
H6 H -0.201(4) 0.187(2) 0.1493(13) 0.041(8) Uiso 1 1 d
H7 H -0.277(4) 0.253(2) 0.2373(16) 0.062(11) Uiso 1 1 d
H8 H -0.117(4) 0.404(2) 0.2513(13) 0.043(9) Uiso 1 1 d
H9 H -0.222(3) 0.368(2) -0.0026(11) 0.033(7) Uiso 1 1 d
H10 H -0.305(4) 0.553(2) 0.0003(12) 0.039(8) Uiso 1 1 d
H11 H -0.132(3) 0.6258(19) 0.0819(10) 0.024(6) Uiso 1 1 d
H12 H 0.250(3) 0.201(2) 0.0428(11) 0.028(7) Uiso 1 1 d
H13 H 0.555(4) 0.247(2) 0.0712(13) 0.048(9) Uiso 1 1 d
H14 H 0.530(3) 0.393(2) 0.1308(11) 0.031(7) Uiso 1 1 d
H15 H 0.103(3) 0.7186(18) 0.1197(10) 0.019(6) Uiso 1 1 d
H16 H 0.543(4) 0.721(2) 0.0606(13) 0.044(9) Uiso 1 1 d
H17 H 0.494(3) 0.556(2) 0.0993(11) 0.033(7) Uiso 1 1 d
H18A H 0.282(5) 0.854(3) 0.0305(19) 0.079(13) Uiso 1 1 d
H18B H 0.166(5) 0.873(3) 0.0731(14) 0.060(10) Uiso 1 1 d
H18C H 0.361(4) 0.896(2) 0.0834(13) 0.048(9) 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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
N9 Mo O1 102.32(8)
N9 Mo N3 90.16(8)
O1 Mo N3 162.09(7)
N9 Mo C2 91.85(9)
O1 Mo C2 38.91(7)
N3 Mo C2 155.04(8)
N9 Mo N7 90.11(8)
O1 Mo N7 80.64(6)
N3 Mo N7 86.61(6)
C2 Mo N7 118.25(8)
N9 Mo N1 93.04(9)
O1 Mo N1 115.54(6)
N3 Mo N1 75.99(7)
C2 Mo N1 79.06(8)
N7 Mo N1 162.31(7)
N9 Mo N5 174.91(8)
O1 Mo N5 82.76(6)
N3 Mo N5 84.82(6)
C2 Mo N5 92.34(8)
N7 Mo N5 90.45(7)
N1 Mo N5 84.92(7)
O4 S O5 116.02(18)
O4 S O3 115.18(19)
O5 S O3 114.52(14)
O4 S C19 102.87(17)
O5 S C19 103.57(14)
O3 S C19 101.94(14)
C2 O1 C5 121.6(2)
C2 O1 Mo 72.63(11)
C5 O1 Mo 128.83(15)
C8 N1 N2 107.0(2)
C8 N1 Mo 132.22(19)
N2 N1 Mo 120.77(14)
C6 N2 N1 108.6(2)
C6 N2 B 129.6(2)
N1 N2 B 120.26(17)
C11 N3 N4 106.65(18)
C11 N3 Mo 132.00(15)
N4 N3 Mo 121.33(13)
C9 N4 N3 109.31(18)
C9 N4 B 130.00(19)
N3 N4 B 120.18(17)
C14 N5 N6 106.16(18)
C14 N5 Mo 134.49(15)
N6 N5 Mo 119.35(13)
C12 N6 N5 109.45(19)
C12 N6 B 129.6(2)
N5 N6 B 120.90(17)
C15 N7 C17 105.43(18)
C15 N7 Mo 122.75(15)
C17 N7 Mo 131.81(14)
C15 N8 C16 107.80(19)
C15 N8 C18 125.0(2)
C16 N8 C18 127.2(2)
O2 N9 Mo 176.1(2)
O1 C2 C4 111.1(2)
O1 C2 C3 114.7(2)
C4 C2 C3 114.2(2)
O1 C2 Mo 68.46(10)
C4 C2 Mo 120.11(17)
C3 C2 Mo 119.32(18)
N2 C6 C7 109.1(3)
C6 C7 C8 105.1(2)
N1 C8 C7 110.2(3)
N4 C9 C10 108.8(2)
C9 C10 C11 104.9(2)
N3 C11 C10 110.3(2)
N6 C12 C13 109.0(2)
C12 C13 C14 105.0(2)
N5 C14 C13 110.4(2)
N7 C15 N8 110.9(2)
C17 C16 N8 106.4(2)
C16 C17 N7 109.5(2)
F2 C19 F1 107.5(3)
F2 C19 F3 105.6(3)
F1 C19 F3 107.8(3)
F2 C19 S 112.7(2)
F1 C19 S 111.5(2)
F3 C19 S 111.4(2)
N6 B N2 109.87(19)
N6 B N4 108.82(18)
N2 B N4 105.88(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo N9 1.7570(19)
Mo O1 2.1259(16)
Mo N3 2.1802(18)
Mo C2 2.181(2)
Mo N7 2.1840(18)
Mo N1 2.1861(18)
Mo N5 2.2493(17)
S O4 1.416(2)
S O5 1.424(2)
S O3 1.434(2)
S C19 1.813(3)
F1 C19 1.322(4)
F2 C19 1.319(3)
F3 C19 1.329(4)
O1 C2 1.436(3)
O1 C5 1.457(3)
O2 N9 1.193(3)
N1 C8 1.332(3)
N1 N2 1.364(3)
N2 C6 1.352(3)
N2 B 1.534(3)
N3 C11 1.338(3)
N3 N4 1.359(2)
N4 C9 1.348(3)
N4 B 1.543(3)
N5 C14 1.341(3)
N5 N6 1.367(2)
N6 C12 1.342(3)
N6 B 1.531(3)
N7 C15 1.332(3)
N7 C17 1.382(3)
N8 C15 1.336(3)
N8 C16 1.369(3)
N8 C18 1.469(3)
C2 C4 1.498(3)
C2 C3 1.505(4)
C6 C7 1.362(5)
C7 C8 1.390(4)
C9 C10 1.370(4)
C10 C11 1.390(3)
C12 C13 1.367(4)
C13 C14 1.389(3)
C16 C17 1.350(3)
