#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:18:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179809 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/05/7010555.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_7010555
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            'C24 H32 Mo Te'
_chemical_formula_weight         544.04
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.665(2)
_cell_length_b                   16.169(3)
_cell_length_c                   16.242(3)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.69
_cell_measurement_theta_min      5.18
_cell_volume                     2271.5(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3731
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        8.99
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.841
_exptl_absorpt_correction_T_max  0.2558
_exptl_absorpt_correction_T_min  0.2304
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.2_mm
_exptl_crystal_size_mid          0.5_mm
_exptl_crystal_size_min          0.7_mm
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00000(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_obs          0.0514
_refine_ls_shift/esd_max         -2.063
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0566P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1276
_refine_ls_wR_factor_obs         0.1094
_reflns_number_observed          2005
_reflns_number_total             2950
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b100372k.txt
_cod_data_source_block           moph10
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.0000P] 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^)+(0.0566P)^2^+0.0000P] 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      P2(1)/c
_cod_database_code               7010555
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo Mo 0.96025(9) 0.31604(5) 0.23478(5) 0.0372(3) Uani 1 d . .
Te Te 0.91632(8) 0.14863(4) 0.19644(5) 0.0557(3) Uani 1 d . .
C11 C 0.8298(10) 0.3041(6) 0.3561(5) 0.042(2) Uani 1 d . .
C12 C 0.8807(11) 0.3871(6) 0.3434(5) 0.041(2) Uani 1 d . .
H12A H 0.8138(11) 0.4360(6) 0.3401(5) 0.050 Uiso 1 calc R .
C13 C 1.0431(12) 0.3884(7) 0.3486(5) 0.057(3) Uani 1 d . .
H13A H 1.1071(12) 0.4384(7) 0.3487(5) 0.068 Uiso 1 calc R .
C14 C 1.0982(12) 0.3081(8) 0.3623(6) 0.058(3) Uani 1 d . .
H14A H 1.2063(12) 0.2913(8) 0.3725(6) 0.070 Uiso 1 calc R .
C15 C 0.9654(13) 0.2572(6) 0.3669(6) 0.051(3) Uani 1 d . .
H15A H 0.9683(13) 0.1977(6) 0.3781(6) 0.061 Uiso 1 calc R .
C16 C 0.6655(12) 0.2788(7) 0.3711(6) 0.055(3) Uani 1 d . .
C17 C 0.6244(14) 0.3203(7) 0.4521(7) 0.084(4) Uani 1 d . .
H17A H 0.6957(14) 0.3025(7) 0.4961(7) 0.126 Uiso 1 calc R .
H17B H 0.5212(14) 0.3050(7) 0.4645(7) 0.126 Uiso 1 calc R .
H17C H 0.6304(14) 0.3793(7) 0.4464(7) 0.126 Uiso 1 calc R .
C18 C 0.5567(13) 0.3052(10) 0.3015(7) 0.106(5) Uani 1 d . .
H18A H 0.4536(13) 0.2885(10) 0.3124(7) 0.160 Uiso 1 calc R .
H18B H 0.5861(13) 0.2798(10) 0.2514(7) 0.160 Uiso 1 calc R .
H18C H 0.5604(13) 0.3643(10) 0.2959(7) 0.160 Uiso 1 calc R .
C19 C 0.6528(13) 0.1858(7) 0.3844(7) 0.074(3) Uani 1 d . .
H19A H 0.7233(13) 0.1693(7) 0.4293(7) 0.111 Uiso 1 calc R .
H19B H 0.6781(13) 0.1572(7) 0.3351(7) 0.111 Uiso 1 calc R .
H19C H 0.5491(13) 0.1722(7) 0.3972(7) 0.111 Uiso 1 calc R .
C21 C 1.0543(10) 0.3833(6) 0.1170(5) 0.039(2) Uani 1 d . .
C22 C 0.9695(12) 0.4396(6) 0.1623(5) 0.044(2) Uani 1 d . .
H22A H 1.0092(12) 0.4921(6) 0.1850(5) 0.053 Uiso 1 calc R .
C23 C 0.8130(11) 0.4122(6) 0.1636(6) 0.050(3) Uani 1 d . .
H23A H 0.7280(11) 0.4437(6) 0.1856(6) 0.059 Uiso 1 calc R .
C24 C 0.7975(12) 0.3374(7) 0.1205(6) 0.053(3) Uani 1 d . .
H24A H 0.7013(12) 0.3077(7) 0.1055(6) 0.064 Uiso 1 calc R .
C25 C 0.9513(11) 0.3187(6) 0.0931(5) 0.041(2) Uani 1 d . .
H25A H 0.9762(11) 0.2719(6) 0.0579(5) 0.049 Uiso 1 calc R .
C26 C 1.2163(10) 0.3949(6) 0.0905(6) 0.049(3) Uani 1 d . .
C27 C 1.2043(12) 0.4466(8) 0.0114(6) 0.083(4) Uani 1 d . .
H27A H 1.3059(12) 0.4554(8) -0.0076(6) 0.124 Uiso 1 calc R .
H27B H 1.1576(12) 0.4989(8) 0.0224(6) 0.124 Uiso 1 calc R .
H27C H 1.1421(12) 0.4177(8) -0.0302(6) 0.124 Uiso 1 calc R .
C28 C 1.2960(12) 0.3116(7) 0.0739(7) 0.066(3) Uani 1 d . .
H28A H 1.3987(12) 0.3216(7) 0.0572(7) 0.099 Uiso 1 calc R .
H28B H 1.2378(12) 0.2825(7) 0.0309(7) 0.099 Uiso 1 calc R .
H28C H 1.3010(12) 0.2788(7) 0.1233(7) 0.099 Uiso 1 calc R .
C29 C 1.3147(12) 0.4428(7) 0.1556(7) 0.070(3) Uani 1 d . .
H29A H 1.4174(12) 0.4495(7) 0.1374(7) 0.105 Uiso 1 calc R .
H29B H 1.3191(12) 0.4129(7) 0.2067(7) 0.105 Uiso 1 calc R .
H29C H 1.2695(12) 0.4962(7) 0.1636(7) 0.105 Uiso 1 calc R .
C1 C 1.1379(12) 0.1119(6) 0.1566(6) 0.048(2) Uani 1 d . .
C2 C 1.1507(13) 0.0902(6) 0.0761(6) 0.060(3) Uani 1 d . .
H2A H 1.0637(13) 0.0912(6) 0.0397(6) 0.073 Uiso 1 calc R .
C3 C 1.2927(17) 0.0665(7) 0.0478(8) 0.083(4) Uani 1 d . .
H3A H 1.3020(17) 0.0527(7) -0.0072(8) 0.100 Uiso 1 calc R .
C4 C 1.4165(16) 0.0640(7) 0.1024(11) 0.086(5) Uani 1 d . .
H4A H 1.5117(16) 0.0482(7) 0.0840(11) 0.104 Uiso 1 calc R .
C5 C 1.4065(14) 0.0841(8) 0.1840(9) 0.083(4) Uani 1 d . .
H5A H 1.4938(14) 0.0818(8) 0.2201(9) 0.100 Uiso 1 calc R .
C6 C 1.2659(14) 0.1078(6) 0.2123(7) 0.059(3) Uani 1 d . .
H6A H 1.2570(14) 0.1209(6) 0.2676(7) 0.071 Uiso 1 calc R .
H H 1.1604(115) 0.2795(56) 0.2207(53) 0.075(31) 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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
C12 Mo C13 36.2(3) . . ?
C12 Mo C23 82.0(3) . . ?
C13 Mo C23 101.6(4) . . ?
C12 Mo C24 110.9(3) . . ?
C13 Mo C24 137.1(4) . . ?
C23 Mo C24 35.7(3) . . ?
C12 Mo C25 141.5(3) . . ?
C13 Mo C25 142.8(4) . . ?
C23 Mo C25 59.7(3) . . ?
C24 Mo C25 37.1(3) . . ?
C12 Mo C22 88.9(3) . . ?
C13 Mo C22 87.2(4) . . ?
C23 Mo C22 36.1(3) . . ?
C24 Mo C22 59.8(4) . . ?
C25 Mo C22 58.4(3) . . ?
C12 Mo C14 59.7(3) . . ?
C13 Mo C14 35.3(4) . . ?
C23 Mo C14 136.8(4) . . ?
C24 Mo C14 170.6(4) . . ?
C25 Mo C14 151.1(3) . . ?
C22 Mo C14 117.8(4) . . ?
C12 Mo C11 36.3(3) . . ?
C13 Mo C11 60.0(3) . . ?
C23 Mo C11 101.5(3) . . ?
C24 Mo C11 113.0(3) . . ?
C25 Mo C11 148.9(3) . . ?
C22 Mo C11 122.1(3) . . ?
C14 Mo C11 59.7(3) . . ?
C12 Mo C15 58.6(3) . . ?
C13 Mo C15 58.4(4) . . ?
C23 Mo C15 136.0(3) . . ?
C24 Mo C15 141.3(4) . . ?
C25 Mo C15 157.1(3) . . ?
C22 Mo C15 144.4(3) . . ?
C14 Mo C15 35.4(3) . . ?
C11 Mo C15 34.8(3) . . ?
C12 Mo C21 122.1(3) . . ?
C13 Mo C21 108.2(3) . . ?
C23 Mo C21 59.4(3) . . ?
C24 Mo C21 60.3(3) . . ?
C25 Mo C21 35.1(3) . . ?
C22 Mo C21 34.7(3) . . ?
C14 Mo C21 123.8(3) . . ?
C11 Mo C21 156.8(3) . . ?
C15 Mo C21 158.4(4) . . ?
C12 Mo Te 128.7(2) . . ?
C13 Mo Te 135.4(3) . . ?
C23 Mo Te 118.8(3) . . ?
C24 Mo Te 84.0(3) . . ?
C25 Mo Te 78.4(2) . . ?
C22 Mo Te 136.7(2) . . ?
C14 Mo Te 101.5(3) . . ?
C11 Mo Te 92.4(2) . . ?
C15 Mo Te 78.8(2) . . ?
C21 Mo Te 108.1(2) . . ?
C1 Te Mo 102.9(3) . . ?
C15 C11 C12 105.2(8) . . ?
C15 C11 C16 128.5(9) . . ?
C12 C11 C16 125.3(8) . . ?
C15 C11 Mo 72.9(5) . . ?
C12 C11 Mo 68.4(5) . . ?
C16 C11 Mo 131.6(7) . . ?
C13 C12 C11 108.8(9) . . ?
C13 C12 Mo 72.7(5) . . ?
C11 C12 Mo 75.3(5) . . ?
C14 C13 C12 109.1(10) . . ?
C14 C13 Mo 74.8(6) . . ?
C12 C13 Mo 71.1(5) . . ?
C13 C14 C15 106.1(9) . . ?
C13 C14 Mo 69.8(6) . . ?
C15 C14 Mo 72.8(6) . . ?
C11 C15 C14 110.8(9) . . ?
C11 C15 Mo 72.3(5) . . ?
C14 C15 Mo 71.8(6) . . ?
C18 C16 C11 111.0(9) . . ?
C18 C16 C19 110.0(10) . . ?
C11 C16 C19 111.5(8) . . ?
C18 C16 C17 110.8(10) . . ?
C11 C16 C17 106.8(9) . . ?
C19 C16 C17 106.6(8) . . ?
C22 C21 C25 106.3(8) . . ?
C22 C21 C26 126.5(9) . . ?
C25 C21 C26 126.8(8) . . ?
C22 C21 Mo 70.2(5) . . ?
C25 C21 Mo 69.1(5) . . ?
C26 C21 Mo 131.0(6) . . ?
C21 C22 C23 109.5(9) . . ?
C21 C22 Mo 75.1(5) . . ?
C23 C22 Mo 70.3(5) . . ?
C24 C23 C22 108.8(8) . . ?
C24 C23 Mo 72.5(5) . . ?
C22 C23 Mo 73.6(5) . . ?
C23 C24 C25 105.6(9) . . ?
C23 C24 Mo 71.9(5) . . ?
C25 C24 Mo 71.8(5) . . ?
C21 C25 C24 109.6(8) . . ?
C21 C25 Mo 75.8(5) . . ?
C24 C25 Mo 71.1(5) . . ?
C21 C26 C27 106.9(8) . . ?
C21 C26 C29 110.9(8) . . ?
C27 C26 C29 108.1(8) . . ?
C21 C26 C28 112.0(8) . . ?
C27 C26 C28 109.7(8) . . ?
C29 C26 C28 109.0(8) . . ?
C2 C1 C6 120.2(10) . . ?
C2 C1 Te 119.1(8) . . ?
C6 C1 Te 120.7(7) . . ?
C1 C2 C3 120.7(12) . . ?
C4 C3 C2 118.3(12) . . ?
C3 C4 C5 122.2(12) . . ?
C4 C5 C6 119.6(12) . . ?
C5 C6 C1 118.9(10) . . ?
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 C12 2.247(8) . ?
Mo C13 2.268(9) . ?
Mo C23 2.281(9) . ?
Mo C24 2.289(10) . ?
Mo C25 2.299(8) . ?
Mo C22 2.324(8) . ?
Mo C14 2.332(10) . ?
Mo C11 2.337(9) . ?
Mo C15 2.345(9) . ?
Mo C21 2.386(8) . ?
Mo Te 2.7985(11) . ?
Te C1 2.146(10) . ?
C11 C15 1.401(13) . ?
C11 C12 1.431(13) . ?
C11 C16 1.514(13) . ?
C12 C13 1.405(13) . ?
C13 C14 1.40(2) . ?
C14 C15 1.420(14) . ?
C16 C18 1.490(15) . ?
C16 C19 1.53(2) . ?
C16 C17 1.539(14) . ?
C21 C22 1.406(12) . ?
C21 C25 1.413(12) . ?
C21 C26 1.504(12) . ?
C22 C23 1.428(13) . ?
C23 C24 1.401(13) . ?
C24 C25 1.461(13) . ?
C26 C27 1.531(12) . ?
C26 C29 1.529(13) . ?
C26 C28 1.545(14) . ?
C1 C2 1.366(12) . ?
C1 C6 1.389(14) . ?
C2 C3 1.392(15) . ?
C3 C4 1.35(2) . ?
C4 C5 1.37(2) . ?
C5 C6 1.382(15) . ?
