#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:18:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179809 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/05/7010563.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_7010563
loop_
_publ_author_name
'Shin, Jun Ho'
'Savage, William'
'Murphy, Vincent J.'
'Bonanno, Jeffrey B.'
'Churchill, David G.'
'Parkin, Gerard'
_publ_section_title
;
 The syntheses, structures and reactivity of
 bis(tert-butylcyclopentadienyl)molybdenum derivatives: nitrogen
 alkylation of an η2-acetonitrile ligand and influence of the
 chalcogen on the barrier to inversion of chalcogenoether adducts
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1732
_journal_paper_doi               10.1039/b100372k
_journal_year                    2001
_chemical_formula_sum            'C18 H28 Mo'
_chemical_formula_weight         340.34
_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                79.229(3)
_cell_angle_beta                 73.725(3)
_cell_angle_gamma                66.888(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1787(13)
_cell_length_b                   10.2650(16)
_cell_length_c                   11.3123(17)
_cell_measurement_temperature    243(2)
_cell_volume                     835.3(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      243(2)
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  '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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5668
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.9268
_exptl_absorpt_correction_T_min  0.8609
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0096(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0399P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                3128
_reflns_number_total             3619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100372k.txt
_cod_data_source_block           h2s10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               7010563
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo 0.44606(3) 0.39451(2) 0.291516(17) 0.02870(9) Uani 1 1 d . . .
H1 H 0.264(3) 0.396(3) 0.264(2) 0.037(7) Uiso 1 1 d . . .
H2 H 0.305(4) 0.388(3) 0.424(3) 0.056(8) Uiso 1 1 d . . .
C11 C 0.4737(3) 0.1620(2) 0.2713(2) 0.0323(5) Uani 1 1 d . . .
C12 C 0.5052(4) 0.1647(3) 0.3877(2) 0.0372(6) Uani 1 1 d . . .
H12A H 0.4343 0.1386 0.4686 0.045 Uiso 1 1 calc R . .
C13 C 0.6586(4) 0.2046(3) 0.3706(3) 0.0417(6) Uani 1 1 d . . .
H13A H 0.7180 0.2048 0.4357 0.050 Uiso 1 1 calc R . .
C14 C 0.7239(4) 0.2266(3) 0.2406(3) 0.0409(6) Uani 1 1 d . . .
H14A H 0.8380 0.2445 0.1998 0.049 Uiso 1 1 calc R . .
C15 C 0.6097(4) 0.2023(3) 0.1789(2) 0.0368(6) Uani 1 1 d . . .
H15A H 0.6295 0.2024 0.0884 0.044 Uiso 1 1 calc R . .
C16 C 0.3413(4) 0.1032(3) 0.2493(2) 0.0379(6) Uani 1 1 d . . .
C17 C 0.4435(4) -0.0579(3) 0.2430(3) 0.0535(8) Uani 1 1 d . . .
H17A H 0.5503 -0.0753 0.1748 0.080 Uiso 1 1 calc R . .
H17B H 0.3635 -0.1006 0.2305 0.080 Uiso 1 1 calc R . .
H17C H 0.4813 -0.0995 0.3198 0.080 Uiso 1 1 calc R . .
C18 C 0.1714(4) 0.1289(4) 0.3551(3) 0.0580(8) Uani 1 1 d . . .
H18A H 0.2073 0.0859 0.4322 0.087 Uiso 1 1 calc R . .
H18B H 0.0924 0.0867 0.3401 0.087 Uiso 1 1 calc R . .
H18C H 0.1064 0.2303 0.3601 0.087 Uiso 1 1 calc R . .
C19 C 0.2845(5) 0.1675(3) 0.1260(3) 0.0583(8) Uani 1 1 d . . .
H19A H 0.2166 0.2688 0.1297 0.087 Uiso 1 1 calc R . .
H19B H 0.2083 0.1223 0.1116 0.087 Uiso 1 1 calc R . .
H19C H 0.3927 0.1519 0.0591 0.087 Uiso 1 1 calc R . .
C21 C 0.2603(3) 0.6288(2) 0.2393(2) 0.0315(5) Uani 1 1 d . . .
C22 C 0.2997(4) 0.6231(3) 0.3555(2) 0.0367(6) Uani 1 1 d . . .
H22A H 0.2070 0.6490 0.4336 0.044 Uiso 1 1 calc R . .
C23 C 0.4909(4) 0.5813(3) 0.3415(2) 0.0402(6) Uani 1 1 d . . .
H23A H 0.5539 0.5787 0.4054 0.048 Uiso 1 1 calc R . .
C24 C 0.5716(4) 0.5611(3) 0.2145(2) 0.0377(6) Uani 1 1 d . . .
H24A H 0.7021 0.5419 0.1746 0.045 Uiso 1 1 calc R . .
C25 C 0.4318(3) 0.5892(3) 0.1516(2) 0.0344(5) Uani 1 1 d . . .
H25A H 0.4491 0.5906 0.0613 0.041 Uiso 1 1 calc R . .
C26 C 0.0712(4) 0.6884(3) 0.2123(3) 0.0412(6) Uani 1 1 d . . .
C27 C 0.0708(4) 0.6302(4) 0.0969(3) 0.0567(8) Uani 1 1 d . . .
H27A H 0.1626 0.6488 0.0277 0.085 Uiso 1 1 calc R . .
H27B H -0.0485 0.6764 0.0777 0.085 Uiso 1 1 calc R . .
H27C H 0.0980 0.5285 0.1125 0.085 Uiso 1 1 calc R . .
C28 C -0.0706(4) 0.6542(4) 0.3214(3) 0.0587(8) Uani 1 1 d . . .
H28A H -0.0384 0.5520 0.3362 0.088 Uiso 1 1 calc R . .
H28B H -0.1901 0.6972 0.3023 0.088 Uiso 1 1 calc R . .
H28C H -0.0729 0.6919 0.3946 0.088 Uiso 1 1 calc R . .
C29 C 0.0202(5) 0.8505(3) 0.1883(4) 0.0752(11) Uani 1 1 d . . .
H29A H 0.0172 0.8885 0.2615 0.113 Uiso 1 1 calc R . .
H29B H -0.0991 0.8933 0.1688 0.113 Uiso 1 1 calc R . .
H29C H 0.1103 0.8720 0.1193 0.113 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1 Mo H2 72.7(13) . . ?
H1 Mo C14 125.3(9) . . ?
H2 Mo C14 123.1(10) . . ?
H1 Mo C24 124.8(9) . . ?
H2 Mo C24 127.2(10) . . ?
C14 Mo C24 88.93(10) . . ?
H1 Mo C13 126.4(9) . . ?
H2 Mo C13 87.2(10) . . ?
C14 Mo C13 36.74(10) . . ?
C24 Mo C13 107.17(10) . . ?
H1 Mo C23 126.8(9) . . ?
H2 Mo C23 91.3(10) . . ?
C14 Mo C23 106.16(10) . . ?
C24 Mo C23 36.52(9) . . ?
C13 Mo C23 102.07(10) . . ?
H1 Mo C15 89.1(9) . . ?
H2 Mo C15 123.1(10) . . ?
C14 Mo C15 36.73(10) . . ?
C24 Mo C15 107.75(10) . . ?
C13 Mo C15 61.12(10) . . ?
C23 Mo C15 138.03(10) . . ?
H1 Mo C25 88.7(9) . . ?
H2 Mo C25 126.8(10) . . ?
C14 Mo C25 108.51(9) . . ?
C24 Mo C25 36.45(9) . . ?
C13 Mo C25 139.25(10) . . ?
C23 Mo C25 60.72(9) . . ?
C15 Mo C25 105.36(9) . . ?
H1 Mo C22 91.7(9) . . ?
H2 Mo C22 71.6(10) . . ?
C14 Mo C22 142.03(10) . . ?
C24 Mo C22 59.63(10) . . ?
C13 Mo C22 128.71(9) . . ?
C23 Mo C22 35.88(10) . . ?
C15 Mo C22 164.61(9) . . ?
C25 Mo C22 59.30(9) . . ?
H1 Mo C12 91.2(9) . . ?
H2 Mo C12 67.3(10) . . ?
C14 Mo C12 59.81(10) . . ?
C24 Mo C12 143.03(10) . . ?
C13 Mo C12 35.89(9) . . ?
C23 Mo C12 129.47(9) . . ?
C15 Mo C12 59.52(9) . . ?
C25 Mo C12 164.88(9) . . ?
C22 Mo C12 135.80(9) . . ?
H1 Mo C21 69.6(9) . . ?
H2 Mo C21 91.6(10) . . ?
C14 Mo C21 144.23(9) . . ?
C24 Mo C21 60.13(9) . . ?
C13 Mo C21 162.27(9) . . ?
C23 Mo C21 60.26(9) . . ?
C15 Mo C21 132.30(9) . . ?
C25 Mo C21 35.78(8) . . ?
C22 Mo C21 35.43(8) . . ?
C12 Mo C21 155.30(9) . . ?
H1 Mo C11 69.8(9) . . ?
H2 Mo C11 88.0(10) . . ?
C14 Mo C11 60.19(9) . . ?
C24 Mo C11 143.60(9) . . ?
C13 Mo C11 60.15(9) . . ?
C23 Mo C11 162.22(9) . . ?
C15 Mo C11 35.87(9) . . ?
C25 Mo C11 132.09(8) . . ?
C22 Mo C11 156.07(9) . . ?
C12 Mo C11 35.24(8) . . ?
C21 Mo C11 137.52(8) . . ?
C12 C11 C15 107.0(2) . . ?
C12 C11 C16 125.8(2) . . ?
C15 C11 C16 126.5(2) . . ?
C12 C11 Mo 71.32(13) . . ?
C15 C11 Mo 69.33(13) . . ?
C16 C11 Mo 132.06(16) . . ?
C11 C12 C13 109.9(2) . . ?
C11 C12 Mo 73.45(13) . . ?
C13 C12 Mo 70.06(14) . . ?
C12 C13 C14 106.6(2) . . ?
C12 C13 Mo 74.05(14) . . ?
C14 C13 Mo 70.33(14) . . ?
C13 C14 C15 108.8(2) . . ?
C13 C14 Mo 72.93(15) . . ?
C15 C14 Mo 73.24(15) . . ?
C14 C15 C11 107.7(2) . . ?
C14 C15 Mo 70.03(14) . . ?
C11 C15 Mo 74.80(14) . . ?
C11 C16 C18 111.5(2) . . ?
C11 C16 C17 106.4(2) . . ?
C18 C16 C17 108.9(2) . . ?
C11 C16 C19 111.6(2) . . ?
C18 C16 C19 109.6(2) . . ?
C17 C16 C19 108.7(2) . . ?
C22 C21 C25 106.4(2) . . ?
C22 C21 C26 125.8(2) . . ?
C25 C21 C26 127.1(2) . . ?
C22 C21 Mo 71.16(14) . . ?
C25 C21 Mo 69.68(13) . . ?
C26 C21 Mo 131.18(17) . . ?
C23 C22 C21 109.9(2) . . ?
C23 C22 Mo 70.36(14) . . ?
C21 C22 Mo 73.41(13) . . ?
C22 C23 C24 106.5(2) . . ?
C22 C23 Mo 73.77(14) . . ?
C24 C23 Mo 70.50(14) . . ?
C23 C24 C25 108.9(2) . . ?
C23 C24 Mo 72.98(14) . . ?
C25 C24 Mo 73.40(14) . . ?
C24 C25 C21 108.2(2) . . ?
C24 C25 Mo 70.15(13) . . ?
C21 C25 Mo 74.54(13) . . ?
C21 C26 C28 111.7(2) . . ?
C21 C26 C27 111.4(2) . . ?
C28 C26 C27 108.7(2) . . ?
C21 C26 C29 106.5(2) . . ?
C28 C26 C29 109.6(3) . . ?
C27 C26 C29 108.9(3) . . ?
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
Mo H1 1.60(2) . ?
Mo H2 1.62(3) . ?
Mo C14 2.242(3) . ?
Mo C24 2.249(2) . ?
Mo C13 2.277(3) . ?
Mo C23 2.281(3) . ?
Mo C15 2.285(3) . ?
Mo C25 2.291(2) . ?
Mo C22 2.325(2) . ?
Mo C12 2.329(2) . ?
Mo C21 2.355(2) . ?
Mo C11 2.356(2) . ?
C11 C12 1.418(3) . ?
C11 C15 1.431(3) . ?
C11 C16 1.524(3) . ?
C12 C13 1.420(4) . ?
C13 C14 1.425(4) . ?
C14 C15 1.427(4) . ?
C16 C18 1.526(4) . ?
C16 C17 1.537(4) . ?
C16 C19 1.541(4) . ?
C21 C22 1.424(3) . ?
C21 C25 1.428(3) . ?
C21 C26 1.521(4) . ?
C22 C23 1.419(4) . ?
C23 C24 1.419(4) . ?
C24 C25 1.420(3) . ?
C26 C28 1.531(4) . ?
C26 C27 1.535(4) . ?
C26 C29 1.538(4) . ?
