#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:18:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179809 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/05/7010566.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_7010566
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 Se'
_chemical_formula_weight         495.40
_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                 93.070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5880(10)
_cell_length_b                   15.9170(10)
_cell_length_c                   16.169(2)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14.98
_cell_measurement_theta_min      4.39
_cell_volume                     2207.1(4)
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3696
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         1.80
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.248
_exptl_absorpt_correction_T_max  0.3035
_exptl_absorpt_correction_T_min  0.1638
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Dark_Orange
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       Block
_exptl_crystal_F_000             1008
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.0031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_obs          0.0560
_refine_ls_shift/esd_max         -0.015
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0554P)²+9.1960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1568
_refine_ls_wR_factor_obs         0.1247
_reflns_number_observed          2166
_reflns_number_total             3377
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b100372k.txt
_cod_data_source_block           mose10
_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^)+(0.0554P)^2^+9.1960P] 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^)+(0.0554P)^2^+9.1960P] 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               7010566
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 0.98223(10) 0.32051(4) 0.23808(5) 0.0438(3) Uani 1 d . .
Se Se 0.94541(14) 0.16036(6) 0.20520(7) 0.0618(4) Uani 1 d . .
H H 1.1306(71) 0.3086(36) 0.2100(36) 0.016(16) Uiso 1 d . .
C11 C 0.8506(11) 0.3098(5) 0.3607(5) 0.047(2) Uani 1 d . .
C12 C 0.9008(13) 0.3938(6) 0.3473(5) 0.054(3) Uani 1 d . .
H12A H 0.8328(13) 0.4433(6) 0.3438(5) 0.065 Uiso 1 calc R .
C13 C 1.0668(15) 0.3954(7) 0.3482(6) 0.067(3) Uani 1 d . .
H13A H 1.1318(15) 0.4459(7) 0.3471(6) 0.081 Uiso 1 calc R .
C14 C 1.1204(13) 0.3135(8) 0.3651(6) 0.069(3) Uani 1 d . .
H14A H 1.2294(13) 0.2961(8) 0.3746(6) 0.083 Uiso 1 calc R .
C15 C 0.9883(13) 0.2624(6) 0.3721(6) 0.058(3) Uani 1 d . .
H15A H 0.9917(13) 0.2021(6) 0.3842(6) 0.069 Uiso 1 calc R .
C16 C 0.6869(13) 0.2822(6) 0.3763(6) 0.060(3) Uani 1 d . .
C17 C 0.5726(14) 0.3125(10) 0.3076(8) 0.107(5) Uani 1 d . .
H17A H 0.4693(14) 0.2943(10) 0.3188(8) 0.160 Uiso 1 calc R .
H17B H 0.6012(14) 0.2897(10) 0.2556(8) 0.160 Uiso 1 calc R .
H17C H 0.5750(14) 0.3728(10) 0.3051(8) 0.160 Uiso 1 calc R .
C18 C 0.6756(14) 0.1878(6) 0.3850(7) 0.081(4) Uani 1 d . .
H18A H 0.5701(14) 0.1725(6) 0.3948(7) 0.121 Uiso 1 calc R .
H18B H 0.7433(14) 0.1695(6) 0.4307(7) 0.121 Uiso 1 calc R .
H18C H 0.7064(14) 0.1614(6) 0.3350(7) 0.121 Uiso 1 calc R .
C19 C 0.6436(14) 0.3220(7) 0.4578(7) 0.087(4) Uani 1 d . .
H19A H 0.5396(14) 0.3057(7) 0.4698(7) 0.130 Uiso 1 calc R .
H19B H 0.6489(14) 0.3821(7) 0.4534(7) 0.130 Uiso 1 calc R .
H19C H 0.7151(14) 0.3033(7) 0.5017(7) 0.130 Uiso 1 calc R .
C21 C 1.0731(11) 0.3862(5) 0.1180(5) 0.043(2) Uani 1 d . .
C22 C 0.9855(12) 0.4445(5) 0.1639(5) 0.048(2) Uani 1 d . .
H22A H 1.0244(12) 0.4985(5) 0.1855(5) 0.058 Uiso 1 calc R .
C23 C 0.8317(12) 0.4162(6) 0.1666(6) 0.056(3) Uani 1 d . .
H23A H 0.7453(12) 0.4478(6) 0.1887(6) 0.067 Uiso 1 calc R .
C24 C 0.8184(11) 0.3400(6) 0.1262(6) 0.050(2) Uani 1 d . .
H24A H 0.7215(11) 0.3091(6) 0.1132(6) 0.061 Uiso 1 calc R .
C25 C 0.9672(10) 0.3213(5) 0.0964(5) 0.046(2) Uani 1 d . .
H25A H 0.9901(10) 0.2730(5) 0.0614(5) 0.055 Uiso 1 calc R .
C26 C 1.2349(12) 0.4000(6) 0.0892(6) 0.055(3) Uani 1 d . .
C27 C 1.2183(14) 0.4516(7) 0.0096(7) 0.081(4) Uani 1 d . .
H27A H 1.3196(14) 0.4617(7) -0.0108(7) 0.122 Uiso 1 calc R .
H27B H 1.1693(14) 0.5043(7) 0.0208(7) 0.122 Uiso 1 calc R .
H27C H 1.1556(14) 0.4213(7) -0.0313(7) 0.122 Uiso 1 calc R .
C28 C 1.3162(12) 0.3162(6) 0.0709(7) 0.070(3) Uani 1 d . .
H28A H 1.4188(12) 0.3272(6) 0.0527(7) 0.105 Uiso 1 calc R .
H28B H 1.2565(12) 0.2865(6) 0.0283(7) 0.105 Uiso 1 calc R .
H28C H 1.3238(12) 0.2827(6) 0.1203(7) 0.105 Uiso 1 calc R .
C29 C 1.3349(14) 0.4489(7) 0.1529(7) 0.077(3) Uani 1 d . .
H29A H 1.4372(14) 0.4568(7) 0.1330(7) 0.116 Uiso 1 calc R .
H29B H 1.3426(14) 0.4181(7) 0.2040(7) 0.116 Uiso 1 calc R .
H29C H 1.2880(14) 0.5026(7) 0.1619(7) 0.116 Uiso 1 calc R .
C1 C 1.1399(13) 0.1228(5) 0.1659(6) 0.057(3) Uani 1 d . .
C2 C 1.2734(15) 0.1172(6) 0.2181(7) 0.070(3) Uani 1 d . .
H2A H 1.2689(15) 0.1327(6) 0.2734(7) 0.083 Uiso 1 calc R .
C3 C 1.4108(15) 0.0895(7) 0.1896(8) 0.080(3) Uani 1 d . .
H3A H 1.4983(15) 0.0850(7) 0.2259(8) 0.095 Uiso 1 calc R .
C4 C 1.4212(17) 0.0682(7) 0.1085(10) 0.086(4) Uani 1 d . .
H4A H 1.5158(17) 0.0505(7) 0.0891(10) 0.103 Uiso 1 calc R .
C5 C 1.2913(18) 0.0730(6) 0.0555(7) 0.080(4) Uani 1 d . .
H5A H 1.2972(18) 0.0590(6) -0.0001(7) 0.096 Uiso 1 calc R .
C6 C 1.1516(14) 0.0989(6) 0.0855(6) 0.063(3) Uani 1 d . .
H6A H 1.0629(14) 0.1001(6) 0.0499(6) 0.076 Uiso 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'
Se Se -0.0929 2.2259 '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
C13 Mo C24 136.9(4) . . ?
C13 Mo C12 37.0(4) . . ?
C24 Mo C12 110.5(4) . . ?
C13 Mo C23 101.5(4) . . ?
C24 Mo C23 35.5(3) . . ?
C12 Mo C23 81.9(4) . . ?
C13 Mo C25 142.6(4) . . ?
C24 Mo C25 36.5(3) . . ?
C12 Mo C25 141.0(3) . . ?
C23 Mo C25 59.2(3) . . ?
C13 Mo C22 86.9(4) . . ?
C24 Mo C22 59.3(3) . . ?
C12 Mo C22 88.7(3) . . ?
C23 Mo C22 35.5(3) . . ?
C25 Mo C22 58.5(3) . . ?
C13 Mo C14 35.9(4) . . ?
C24 Mo C14 170.3(4) . . ?
C12 Mo C14 59.9(4) . . ?
C23 Mo C14 137.1(4) . . ?
C25 Mo C14 152.3(3) . . ?
C22 Mo C14 118.8(4) . . ?
C13 Mo C11 60.9(4) . . ?
C24 Mo C11 112.4(3) . . ?
C12 Mo C11 36.1(3) . . ?
C23 Mo C11 101.1(3) . . ?
C25 Mo C11 147.6(3) . . ?
C22 Mo C11 121.5(3) . . ?
C14 Mo C11 59.6(4) . . ?
C13 Mo C15 59.0(4) . . ?
C24 Mo C15 140.8(4) . . ?
C12 Mo C15 58.4(3) . . ?
C23 Mo C15 135.7(3) . . ?
C25 Mo C15 157.1(3) . . ?
C22 Mo C15 144.4(3) . . ?
C14 Mo C15 35.0(3) . . ?
C11 Mo C15 34.9(3) . . ?
C13 Mo C21 108.1(3) . . ?
C24 Mo C21 60.1(3) . . ?
C12 Mo C21 122.7(3) . . ?
C23 Mo C21 59.5(3) . . ?
C25 Mo C21 35.1(3) . . ?
C22 Mo C21 35.4(3) . . ?
C14 Mo C21 124.8(4) . . ?
C11 Mo C21 156.9(3) . . ?
C15 Mo C21 159.1(4) . . ?
C13 Mo Se 135.4(3) . . ?
C24 Mo Se 84.7(2) . . ?
C12 Mo Se 128.5(2) . . ?
C23 Mo Se 119.3(3) . . ?
C25 Mo Se 78.6(2) . . ?
C22 Mo Se 136.9(2) . . ?
C14 Mo Se 100.5(3) . . ?
C11 Mo Se 92.4(2) . . ?
C15 Mo Se 78.5(2) . . ?
C21 Mo Se 107.7(2) . . ?
C1 Se Mo 105.8(3) . . ?
C15 C11 C12 105.3(9) . . ?
C15 C11 C16 127.3(8) . . ?
C12 C11 C16 126.3(8) . . ?
C15 C11 Mo 73.1(5) . . ?
C12 C11 Mo 68.9(4) . . ?
C16 C11 Mo 131.3(7) . . ?
C11 C12 C13 109.0(9) . . ?
C11 C12 Mo 75.1(5) . . ?
C13 C12 Mo 70.5(5) . . ?
C14 C13 C12 107.7(9) . . ?
C14 C13 Mo 75.4(6) . . ?
C12 C13 Mo 72.5(6) . . ?
C13 C14 C15 107.2(10) . . ?
C13 C14 Mo 68.7(6) . . ?
C15 C14 Mo 73.9(6) . . ?
C14 C15 C11 110.8(9) . . ?
C14 C15 Mo 71.1(6) . . ?
C11 C15 Mo 72.0(5) . . ?
C11 C16 C18 111.7(8) . . ?
C11 C16 C17 110.9(8) . . ?
C18 C16 C17 110.0(10) . . ?
C11 C16 C19 107.2(9) . . ?
C18 C16 C19 108.2(8) . . ?
C17 C16 C19 108.7(10) . . ?
C25 C21 C22 104.8(8) . . ?
C25 C21 C26 128.6(8) . . ?
C22 C21 C26 126.0(8) . . ?
C25 C21 Mo 69.1(4) . . ?
C22 C21 Mo 69.9(4) . . ?
C26 C21 Mo 131.8(6) . . ?
C23 C22 C21 109.4(8) . . ?
C23 C22 Mo 70.8(5) . . ?
C21 C22 Mo 74.7(4) . . ?
C24 C23 C22 108.8(9) . . ?
C24 C23 Mo 71.4(5) . . ?
C22 C23 Mo 73.7(5) . . ?
C23 C24 C25 107.0(8) . . ?
C23 C24 Mo 73.1(6) . . ?
C25 C24 Mo 73.1(5) . . ?
C21 C25 C24 110.0(8) . . ?
C21 C25 Mo 75.8(5) . . ?
C24 C25 Mo 70.4(5) . . ?
C21 C26 C29 111.2(8) . . ?
C21 C26 C27 107.1(8) . . ?
C29 C26 C27 108.7(9) . . ?
C21 C26 C28 111.6(7) . . ?
C29 C26 C28 109.1(9) . . ?
C27 C26 C28 109.1(9) . . ?
C6 C1 C2 117.5(10) . . ?
C6 C1 Se 120.9(9) . . ?
C2 C1 Se 121.6(8) . . ?
C3 C2 C1 121.1(11) . . ?
C4 C3 C2 120.5(13) . . ?
C3 C4 C5 119.7(12) . . ?
C4 C5 C6 119.3(11) . . ?
C1 C6 C5 121.9(12) . . ?
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 C13 2.232(10) . ?
Mo C24 2.252(9) . ?
Mo C12 2.259(8) . ?
Mo C23 2.273(9) . ?
Mo C25 2.288(8) . ?
Mo C22 2.311(8) . ?
Mo C14 2.318(10) . ?
Mo C11 2.340(8) . ?
Mo C15 2.355(9) . ?
Mo C21 2.373(7) . ?
Mo Se 2.6198(12) . ?
Se C1 1.914(10) . ?
C11 C15 1.407(13) . ?
C11 C12 1.425(12) . ?
C11 C16 1.507(13) . ?
C12 C13 1.425(14) . ?
C13 C14 1.405(15) . ?
C14 C15 1.405(14) . ?
C16 C18 1.514(13) . ?
C16 C17 1.521(15) . ?
C16 C19 1.527(13) . ?
C21 C25 1.409(12) . ?
C21 C22 1.427(12) . ?
C21 C26 1.506(13) . ?
C22 C23 1.399(13) . ?
C23 C24 1.379(13) . ?
C24 C25 1.422(12) . ?
C26 C29 1.519(14) . ?
C26 C27 1.526(12) . ?
C26 C28 1.541(13) . ?
C1 C6 1.363(13) . ?
C1 C2 1.390(14) . ?
C2 C3 1.363(15) . ?
C3 C4 1.36(2) . ?
C4 C5 1.37(2) . ?
C5 C6 1.381(15) . ?
