#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:13:50 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179682 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/04/7000478.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_7000478
loop_
_publ_author_name
'Cross, Warren B.'
'Anderson, James C.'
'Wilson, Claire S.'
_publ_section_title
;
 Nucleophilic reactivity of a d0 molybdenum oxo moiety
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1201
_journal_page_last               1205
_journal_paper_doi               10.1039/b817745g
_journal_year                    2009
_chemical_formula_sum            'C34 H54 Cl Mo N O4'
_chemical_formula_weight         672.17
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.411(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.400(2)
_cell_length_b                   10.8824(14)
_cell_length_c                   21.642(3)
_cell_measurement_reflns_used    3624
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.3
_cell_volume                     3460.8(8)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material  'enCIFer (CCDC, 2003); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21505
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS v2.05'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0427
_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)+(0.0475P)²+1.1945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                5956
_reflns_number_total             7886
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b817745g.txt
_cod_data_source_block           montip
_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      'P 21/n'
_cod_database_code               7000478
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl 0.38312(5) 0.85504(7) 0.23201(3) 0.02652(17) Uani 1 1 d . . .
Mo1 Mo 0.329629(16) 0.88751(2) 0.116340(11) 0.01668(8) Uani 1 1 d . . .
O1 O 0.39801(13) 1.05525(18) 0.14229(9) 0.0215(4) Uani 1 1 d . . .
N1 N 0.22447(16) 0.9397(2) 0.11386(11) 0.0208(5) Uani 1 1 d . . .
C1 C 0.13945(19) 1.0031(3) 0.11093(14) 0.0227(6) Uani 1 1 d . . .
O2 O 0.32283(13) 0.92028(17) 0.02811(9) 0.0192(4) Uani 1 1 d . . .
C2 C 0.0607(2) 0.9207(3) 0.07364(15) 0.0283(7) Uani 1 1 d . . .
H2A H 0.0626 0.8435 0.0972 0.042 Uiso 1 1 calc R . .
H2B H 0.0664 0.9034 0.0306 0.042 Uiso 1 1 calc R . .
H2C H 0.0029 0.9626 0.0692 0.042 Uiso 1 1 calc R . .
O3 O 0.32166(13) 0.71708(17) 0.11008(9) 0.0210(4) Uani 1 1 d . . .
C3 C 0.1384(2) 1.1251(3) 0.07523(17) 0.0326(7) Uani 1 1 d . . .
H3A H 0.1893 1.1764 0.0999 0.049 Uiso 1 1 calc R . .
H3B H 0.0809 1.1680 0.0709 0.049 Uiso 1 1 calc R . .
H3C H 0.1443 1.1089 0.0321 0.049 Uiso 1 1 calc R . .
O4 O 0.47973(13) 0.90239(17) 0.12700(9) 0.0215(4) Uani 1 1 d . . .
C4 C 0.1379(2) 1.0243(4) 0.18015(16) 0.0393(9) Uani 1 1 d . . .
H4A H 0.1388 0.9450 0.2017 0.059 Uiso 1 1 calc R . .
H4B H 0.0826 1.0694 0.1796 0.059 Uiso 1 1 calc R . .
H4C H 0.1915 1.0723 0.2037 0.059 Uiso 1 1 calc R . .
C5 C 0.2568(2) 0.9560(3) -0.02744(13) 0.0206(6) Uani 1 1 d . . .
C6 C 0.2523(2) 1.0800(3) -0.04631(14) 0.0237(6) Uani 1 1 d . . .
C7 C 0.1878(2) 1.1111(3) -0.10453(14) 0.0305(7) Uani 1 1 d . . .
H7A H 0.1827 1.1943 -0.1184 0.037 Uiso 1 1 calc R . .
C8 C 0.1312(2) 1.0243(3) -0.14251(15) 0.0327(8) Uani 1 1 d . . .
H8A H 0.0881 1.0479 -0.1822 0.039 Uiso 1 1 calc R . .
C9 C 0.1371(2) 0.9033(3) -0.12287(14) 0.0299(7) Uani 1 1 d . . .
H9A H 0.0977 0.8443 -0.1495 0.036 Uiso 1 1 calc R . .
C10 C 0.1993(2) 0.8653(3) -0.06508(14) 0.0229(6) Uani 1 1 d . . .
C11 C 0.3162(2) 1.1756(3) -0.00496(15) 0.0254(7) Uani 1 1 d . . .
H11A H 0.3235 1.1551 0.0414 0.030 Uiso 1 1 calc R . .
C12 C 0.2798(3) 1.3067(3) -0.01640(17) 0.0351(8) Uani 1 1 d . . .
H12A H 0.2196 1.3105 -0.0099 0.053 Uiso 1 1 calc R . .
H12B H 0.2750 1.3315 -0.0608 0.053 Uiso 1 1 calc R . .
H12C H 0.3214 1.3623 0.0141 0.053 Uiso 1 1 calc R . .
C13 C 0.4100(2) 1.1659(3) -0.01475(17) 0.0367(8) Uani 1 1 d . . .
H13A H 0.4319 1.0810 -0.0071 0.055 Uiso 1 1 calc R . .
H13B H 0.4525 1.2207 0.0157 0.055 Uiso 1 1 calc R . .
H13C H 0.4060 1.1897 -0.0592 0.055 Uiso 1 1 calc R . .
C14 C 0.2085(2) 0.7326(3) -0.04342(15) 0.0253(7) Uani 1 1 d . . .
H14A H 0.2153 0.7323 0.0040 0.030 Uiso 1 1 calc R . .
C15 C 0.1264(3) 0.6532(3) -0.07611(18) 0.0445(9) Uani 1 1 d . . .
H15A H 0.0715 0.6906 -0.0703 0.067 Uiso 1 1 calc R . .
H15B H 0.1348 0.5710 -0.0567 0.067 Uiso 1 1 calc R . .
H15C H 0.1199 0.6467 -0.1224 0.067 Uiso 1 1 calc R . .
C16 C 0.2954(2) 0.6758(3) -0.05181(17) 0.0375(8) Uani 1 1 d . . .
H16A H 0.3477 0.7281 -0.0305 0.056 Uiso 1 1 calc R . .
H16B H 0.2896 0.6693 -0.0980 0.056 Uiso 1 1 calc R . .
H16C H 0.3046 0.5938 -0.0322 0.056 Uiso 1 1 calc R . .
C17 C 0.3256(2) 0.5974(2) 0.12828(13) 0.0197(6) Uani 1 1 d . . .
C18 C 0.2468(2) 0.5412(3) 0.13555(13) 0.0206(6) Uani 1 1 d . . .
C19 C 0.2537(2) 0.4188(3) 0.15483(14) 0.0279(7) Uani 1 1 d . . .
H19A H 0.2021 0.3787 0.1609 0.033 Uiso 1 1 calc R . .
C20 C 0.3347(2) 0.3540(3) 0.16534(15) 0.0312(8) Uani 1 1 d . . .
H20A H 0.3381 0.2703 0.1783 0.037 Uiso 1 1 calc R . .
C21 C 0.4102(2) 0.4116(3) 0.15682(15) 0.0279(7) Uani 1 1 d . . .
H21A H 0.4652 0.3665 0.1644 0.033 Uiso 1 1 calc R . .
C22 C 0.4081(2) 0.5338(3) 0.13743(13) 0.0211(6) Uani 1 1 d . . .
C23 C 0.1601(2) 0.6131(3) 0.12568(14) 0.0261(6) Uani 1 1 d . . .
H23A H 0.1616 0.6839 0.0966 0.031 Uiso 1 1 calc R . .
C24 C 0.0746(2) 0.5385(4) 0.09352(18) 0.0450(9) Uani 1 1 d . . .
H24A H 0.0783 0.5056 0.0522 0.067 Uiso 1 1 calc R . .
H24B H 0.0210 0.5916 0.0856 0.067 Uiso 1 1 calc R . .
H24C H 0.0697 0.4706 0.1220 0.067 Uiso 1 1 calc R . .
C25 C 0.1563(2) 0.6658(3) 0.19031(15) 0.0299(7) Uani 1 1 d . . .
H25A H 0.2116 0.7136 0.2101 0.045 Uiso 1 1 calc R . .
H25B H 0.1520 0.5984 0.2193 0.045 Uiso 1 1 calc R . .
H25C H 0.1029 0.7192 0.1830 0.045 Uiso 1 1 calc R . .
C26 C 0.4906(2) 0.5946(3) 0.12715(15) 0.0251(7) Uani 1 1 d . . .
H26A H 0.4693 0.6673 0.0984 0.030 Uiso 1 1 calc R . .
C27 C 0.5547(2) 0.6406(3) 0.19034(17) 0.0394(9) Uani 1 1 d . . .
H27A H 0.5218 0.6953 0.2115 0.059 Uiso 1 1 calc R . .
H27B H 0.6050 0.6858 0.1817 0.059 Uiso 1 1 calc R . .
H27C H 0.5791 0.5706 0.2187 0.059 Uiso 1 1 calc R . .
C28 C 0.5411(3) 0.5093(4) 0.0937(2) 0.0488(10) Uani 1 1 d . . .
H28A H 0.5943 0.5520 0.0881 0.073 Uiso 1 1 calc R . .
H28B H 0.5005 0.4854 0.0512 0.073 Uiso 1 1 calc R . .
H28C H 0.5610 0.4357 0.1202 0.073 Uiso 1 1 calc R . .
C29 C 0.47580(19) 1.0141(3) 0.13990(13) 0.0203(6) Uani 1 1 d . . .
C30 C 0.5560(2) 1.0983(3) 0.15302(14) 0.0240(6) Uani 1 1 d . . .
H30A H 0.5339 1.1832 0.1418 0.029 Uiso 1 1 calc R . .
H30B H 0.5928 1.0752 0.1243 0.029 Uiso 1 1 calc R . .
C31 C 0.6182(2) 1.0964(3) 0.22428(15) 0.0268(7) Uani 1 1 d . . .
C32 C 0.5623(2) 1.1223(3) 0.27018(16) 0.0368(8) Uani 1 1 d . . .
H32A H 0.6022 1.1209 0.3150 0.055 Uiso 1 1 calc R . .
H32B H 0.5151 1.0594 0.2646 0.055 Uiso 1 1 calc R . .
H32C H 0.5338 1.2034 0.2606 0.055 Uiso 1 1 calc R . .
C33 C 0.6650(3) 0.9726(3) 0.23972(18) 0.0424(9) Uani 1 1 d . . .
H33A H 0.7040 0.9721 0.2848 0.064 Uiso 1 1 calc R . .
H33B H 0.7023 0.9580 0.2108 0.064 Uiso 1 1 calc R . .
H33C H 0.6191 0.9077 0.2336 0.064 Uiso 1 1 calc R . .
C34 C 0.6892(2) 1.1978(3) 0.23064(18) 0.0388(9) Uani 1 1 d . . .
H34A H 0.7299 1.1997 0.2752 0.058 Uiso 1 1 calc R . .
H34B H 0.6585 1.2773 0.2200 0.058 Uiso 1 1 calc R . .
H34C H 0.7247 1.1813 0.2008 0.058 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'
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N1 Mo1 O3 106.80(10) . . ?
N1 Mo1 O2 97.99(10) . . ?
O3 Mo1 O2 97.49(8) . . ?
N1 Mo1 O1 96.58(10) . . ?
O3 Mo1 O1 154.61(8) . . ?
O2 Mo1 O1 88.75(8) . . ?
N1 Mo1 O4 156.10(10) . . ?
O3 Mo1 O4 97.01(8) . . ?
O2 Mo1 O4 80.64(8) . . ?
O1 Mo1 O4 59.61(7) . . ?
N1 Mo1 Cl 96.18(8) . . ?
O3 Mo1 Cl 85.65(6) . . ?
O2 Mo1 Cl 163.90(6) . . ?
O1 Mo1 Cl 82.05(6) . . ?
O4 Mo1 Cl 83.31(5) . . ?
N1 Mo1 C29 126.80(10) . . ?
O3 Mo1 C29 125.90(9) . . ?
O2 Mo1 C29 83.15(8) . . ?
O1 Mo1 C29 30.29(8) . . ?
O4 Mo1 C29 29.33(8) . . ?
Cl Mo1 C29 82.26(6) . . ?
C29 O1 Mo1 94.86(17) . . ?
C1 N1 Mo1 171.4(2) . . ?
N1 C1 C4 107.8(2) . . ?
N1 C1 C2 107.7(2) . . ?
C4 C1 C2 111.4(3) . . ?
N1 C1 C3 107.7(2) . . ?
C4 C1 C3 111.3(3) . . ?
C2 C1 C3 110.8(2) . . ?
C5 O2 Mo1 136.76(17) . . ?
C17 O3 Mo1 159.95(18) . . ?
C29 O4 Mo1 88.63(17) . . ?
O2 C5 C6 118.9(3) . . ?
O2 C5 C10 118.5(2) . . ?
C6 C5 C10 122.4(3) . . ?
C7 C6 C5 117.1(3) . . ?
C7 C6 C11 121.7(3) . . ?
C5 C6 C11 121.2(3) . . ?
C8 C7 C6 121.7(3) . . ?
C7 C8 C9 119.9(3) . . ?
C8 C9 C10 121.7(3) . . ?
C9 C10 C5 117.1(3) . . ?
C9 C10 C14 122.5(3) . . ?
C5 C10 C14 120.4(3) . . ?
C6 C11 C12 113.7(3) . . ?
C6 C11 C13 110.1(2) . . ?
C12 C11 C13 111.0(3) . . ?
C10 C14 C15 114.3(3) . . ?
C10 C14 C16 110.6(3) . . ?
C15 C14 C16 110.5(3) . . ?
O3 C17 C22 118.3(2) . . ?
O3 C17 C18 118.9(3) . . ?
C22 C17 C18 122.8(3) . . ?
C19 C18 C17 117.3(3) . . ?
C19 C18 C23 121.6(3) . . ?
C17 C18 C23 121.0(3) . . ?
C18 C19 C20 121.2(3) . . ?
C21 C20 C19 119.8(3) . . ?
C20 C21 C22 122.0(3) . . ?
C21 C22 C17 116.8(3) . . ?
C21 C22 C26 121.3(3) . . ?
C17 C22 C26 121.9(3) . . ?
C18 C23 C24 113.3(3) . . ?
C18 C23 C25 109.8(2) . . ?
C24 C23 C25 110.7(3) . . ?
C22 C26 C27 111.3(3) . . ?
C22 C26 C28 112.0(3) . . ?
C27 C26 C28 110.0(3) . . ?
O4 C29 O1 116.8(3) . . ?
O4 C29 C30 123.0(3) . . ?
O1 C29 C30 120.2(3) . . ?
O4 C29 Mo1 62.04(15) . . ?
O1 C29 Mo1 54.85(14) . . ?
C30 C29 Mo1 174.8(2) . . ?
C29 C30 C31 114.1(2) . . ?
C33 C31 C32 110.2(3) . . ?
C33 C31 C34 109.9(3) . . ?
C32 C31 C34 109.6(3) . . ?
C33 C31 C30 110.0(3) . . ?
C32 C31 C30 110.2(3) . . ?
C34 C31 C30 106.9(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
Cl Mo1 2.4157(8) . ?
Mo1 N1 1.702(2) . ?
Mo1 O3 1.8610(19) . ?
Mo1 O2 1.9144(19) . ?
Mo1 O1 2.098(2) . ?
Mo1 O4 2.259(2) . ?
Mo1 C29 2.557(3) . ?
O1 C29 1.294(3) . ?
N1 C1 1.464(4) . ?
C1 C4 1.523(4) . ?
C1 C2 1.529(4) . ?
C1 C3 1.534(4) . ?
O2 C5 1.378(3) . ?
O3 C17 1.357(3) . ?
O4 C29 1.253(3) . ?
C5 C6 1.406(4) . ?
C5 C10 1.410(4) . ?
C6 C7 1.393(4) . ?
C6 C11 1.524(4) . ?
C7 C8 1.378(5) . ?
C8 C9 1.379(5) . ?
C9 C10 1.391(4) . ?
C10 C14 1.512(4) . ?
C11 C12 1.525(4) . ?
C11 C13 1.526(4) . ?
C14 C15 1.521(4) . ?
C14 C16 1.534(4) . ?
C17 C22 1.407(4) . ?
C17 C18 1.409(4) . ?
C18 C19 1.390(4) . ?
C18 C23 1.508(4) . ?
C19 C20 1.392(5) . ?
C20 C21 1.380(4) . ?
C21 C22 1.392(4) . ?
C22 C26 1.507(4) . ?
C23 C24 1.525(4) . ?
C23 C25 1.529(4) . ?
C26 C27 1.513(5) . ?
C26 C28 1.526(4) . ?
C29 C30 1.495(4) . ?
C30 C31 1.553(4) . ?
C31 C33 1.518(5) . ?
C31 C32 1.522(4) . ?
C31 C34 1.531(4) . ?
