#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:18:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179809 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/05/7010561.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_7010561
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 H26 Mo O'
_chemical_formula_weight         354.33
_chemical_name_systematic
; 
? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.21(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.601(3)
_cell_length_b                   6.2830(10)
_cell_length_c                   17.732(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1704.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0131
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            1547
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.9275
_exptl_absorpt_correction_T_min  0.6169
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0012(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   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0293
_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)+(0.0380P)²+1.2461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                1320
_reflns_number_total             1490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100372k.txt
_cod_data_source_block           moo20
_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 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010561
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_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 0.0000 0.20671(6) 0.7500 0.04891(16) Uani 1 2 d S . .
O O 0.0000 -0.0647(5) 0.7500 0.154(3) Uani 1 2 d S . .
C11 C 0.04286(18) 0.2996(4) 0.63438(14) 0.0426(6) Uani 1 1 d . . .
C12 C -0.0312(2) 0.1644(5) 0.61691(16) 0.0573(8) Uani 1 1 d . . .
H12A H -0.0327 0.0312 0.5901 0.080 Uiso 1 1 d R . .
C13 C -0.1034(2) 0.2682(6) 0.6371(2) 0.0726(10) Uani 1 1 d . . .
H13A H -0.1625 0.2169 0.6272 0.080 Uiso 1 1 d R . .
C14 C -0.0766(2) 0.4717(6) 0.66347(17) 0.0602(8) Uani 1 1 d . . .
H14A H -0.1135 0.5815 0.6773 0.080 Uiso 1 1 d R . .
C15 C 0.01171(19) 0.4932(4) 0.66086(15) 0.0472(7) Uani 1 1 d . . .
H15A H 0.0462 0.6196 0.6731 0.080 Uiso 1 1 d R . .
C21 C 0.1311(2) 0.2659(5) 0.61202(18) 0.0538(7) Uani 1 1 d . . .
C22 C 0.1508(3) 0.0292(6) 0.6071(2) 0.0794(11) Uani 1 1 d . . .
H22A H 0.1053 -0.0363 0.5701 0.080 Uiso 1 1 d R . .
H22B H 0.2059 0.0100 0.5916 0.080 Uiso 1 1 d R . .
H22C H 0.1529 -0.0355 0.6565 0.080 Uiso 1 1 d R . .
C23 C 0.1270(3) 0.3681(8) 0.5331(2) 0.0851(12) Uani 1 1 d . . .
H23A H 0.0817 0.3006 0.4964 0.080 Uiso 1 1 d R . .
H23B H 0.1139 0.5168 0.5363 0.080 Uiso 1 1 d R . .
H23C H 0.1819 0.3517 0.5170 0.080 Uiso 1 1 d R . .
C24 C 0.2032(2) 0.3701(7) 0.6705(2) 0.0769(10) Uani 1 1 d . . .
H24A H 0.1908 0.5193 0.6733 0.080 Uiso 1 1 d R . .
H24B H 0.2055 0.3062 0.7200 0.080 Uiso 1 1 d R . .
H24C H 0.2585 0.3517 0.6551 0.080 Uiso 1 1 d 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'
O O 0.0106 0.0060 '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
O Mo C12 83.45(8) . . ?
O Mo C12 83.45(8) . 2_556 ?
C12 Mo C12 166.89(16) . 2_556 ?
O Mo C13 99.48(10) . 2_556 ?
C12 Mo C13 148.94(12) . 2_556 ?
C12 Mo C13 35.02(12) 2_556 2_556 ?
O Mo C13 99.48(10) . . ?
C12 Mo C13 35.02(12) . . ?
C12 Mo C13 148.94(12) 2_556 . ?
C13 Mo C13 161.0(2) 2_556 . ?
O Mo C11 104.39(7) . 2_556 ?
C12 Mo C11 150.81(11) . 2_556 ?
C12 Mo C11 35.29(10) 2_556 2_556 ?
C13 Mo C11 58.64(11) 2_556 2_556 ?
C13 Mo C11 116.01(11) . 2_556 ?
O Mo C11 104.39(7) . . ?
C12 Mo C11 35.29(10) . . ?
C12 Mo C11 150.81(11) 2_556 . ?
C13 Mo C11 116.01(12) 2_556 . ?
C13 Mo C11 58.64(11) . . ?
C11 Mo C11 151.23(14) 2_556 . ?
O Mo C14 133.53(9) . 2_556 ?
C12 Mo C14 134.56(11) . 2_556 ?
C12 Mo C14 57.02(12) 2_556 2_556 ?
C13 Mo C14 34.06(12) 2_556 2_556 ?
C13 Mo C14 126.98(15) . 2_556 ?
C11 Mo C14 57.63(10) 2_556 2_556 ?
C11 Mo C14 101.13(10) . 2_556 ?
O Mo C14 133.53(9) . . ?
C12 Mo C14 57.02(12) . . ?
C12 Mo C14 134.56(11) 2_556 . ?
C13 Mo C14 126.98(15) 2_556 . ?
C13 Mo C14 34.06(12) . . ?
C11 Mo C14 101.13(10) 2_556 . ?
C11 Mo C14 57.63(10) . . ?
C14 Mo C14 92.94(18) 2_556 . ?
O Mo C15 137.90(7) . . ?
C12 Mo C15 56.78(10) . . ?
C12 Mo C15 135.83(11) 2_556 . ?
C13 Mo C15 107.91(12) 2_556 . ?
C13 Mo C15 56.49(12) . . ?
C11 Mo C15 117.02(10) 2_556 . ?
C11 Mo C15 34.61(9) . . ?
C14 Mo C15 79.16(11) 2_556 . ?
C14 Mo C15 33.48(10) . . ?
O Mo C15 137.90(7) . 2_556 ?
C12 Mo C15 135.83(11) . 2_556 ?
C12 Mo C15 56.78(10) 2_556 2_556 ?
C13 Mo C15 56.49(12) 2_556 2_556 ?
C13 Mo C15 107.91(12) . 2_556 ?
C11 Mo C15 34.61(9) 2_556 2_556 ?
C11 Mo C15 117.02(10) . 2_556 ?
C14 Mo C15 33.48(10) 2_556 2_556 ?
C14 Mo C15 79.16(11) . 2_556 ?
C15 Mo C15 84.19(13) . 2_556 ?
C12 C11 C15 105.6(3) . . ?
C12 C11 C21 126.9(3) . . ?
C15 C11 C21 126.2(3) . . ?
C12 C11 Mo 71.59(15) . . ?
C15 C11 Mo 75.58(15) . . ?
C21 C11 Mo 128.22(19) . . ?
C13 C12 C11 108.9(3) . . ?
C13 C12 Mo 73.1(2) . . ?
C11 C12 Mo 73.13(15) . . ?
C14 C13 C12 107.9(3) . . ?
C14 C13 Mo 75.74(19) . . ?
C12 C13 Mo 71.88(19) . . ?
C15 C14 C13 108.1(3) . . ?
C15 C14 Mo 73.60(16) . . ?
C13 C14 Mo 70.19(19) . . ?
C14 C15 C11 109.4(3) . . ?
C14 C15 Mo 72.92(17) . . ?
C11 C15 Mo 69.80(14) . . ?
C11 C21 C24 110.5(3) . . ?
C11 C21 C22 110.7(3) . . ?
C24 C21 C22 109.2(3) . . ?
C11 C21 C23 107.5(3) . . ?
C24 C21 C23 109.7(3) . . ?
C22 C21 C23 109.3(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 O 1.705(4) . ?
Mo C12 2.330(3) . ?
Mo C12 2.330(3) 2_556 ?
Mo C13 2.346(4) 2_556 ?
Mo C13 2.346(4) . ?
Mo C11 2.350(2) 2_556 ?
Mo C11 2.350(2) . ?
Mo C14 2.417(3) 2_556 ?
Mo C14 2.417(3) . ?
Mo C15 2.426(3) . ?
Mo C15 2.426(3) 2_556 ?
C11 C12 1.419(4) . ?
C11 C15 1.423(4) . ?
C11 C21 1.520(4) . ?
C12 C13 1.407(5) . ?
C13 C14 1.397(5) . ?
C14 C15 1.395(4) . ?
C21 C24 1.522(5) . ?
C21 C22 1.525(4) . ?
C21 C23 1.530(4) . ?
