#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:02:54 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180220 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/06/7110612.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7110612
loop_
_publ_author_name
'Bandyopadhyay, Ratna'
'Biswas, Sudeb'
'Bhattacharyya, Ramgopal'
'Guha, Subhadra'
'Mukherjee, Alok K.'
_publ_section_title
;
 Novel oxo-peroxo molybdenum(VI) complexes incorporating 8-quinolinol:
 synthesis, structure and catalytic uses in the environmentally benign and
 cost-effective oxidation method of methyl benzenes: Ar(CH3)n (n = 1, 2)
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1627
_journal_paper_doi               10.1039/a904440j
_journal_year                    1999
_chemical_formula_sum            'C19 H14 Cl2 Mo N2 O5'
_chemical_formula_weight         517.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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
_cell_angle_alpha                117.700(10)
_cell_angle_beta                 90.140(10)
_cell_angle_gamma                105.080(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7912(10)
_cell_length_b                   10.6430(10)
_cell_length_c                   10.9638(10)
_cell_measurement_temperature    293(2)
_cell_volume                     966.5(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71093
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3552
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.990
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_F_000             516
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.099
_refine_ls_goodness_of_fit_obs   1.124
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3359
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.166
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_obs          0.0414
_refine_ls_shift/esd_max         -0.025
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s²(Fo²)+( 0.0935P)²+0.4574P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1235
_refine_ls_wR_factor_obs         0.1190
_reflns_number_observed          3006
_reflns_number_total             3359
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904440jsup1.cif
_cod_data_source_block           shelx93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0935P)^2^+0.4574P] 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^)+( 0.0935P)^2^+0.4574P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7110612
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cl1 Cl 0.4090(4) -0.2361(4) -0.0846(3) 0.1062(8) Uiso 0.75 d PD 1
Cl2 Cl 0.5449(5) -0.4587(5) -0.2096(5) 0.0905(11) Uiso 0.45 d PD 1
Cl3 Cl 0.4867(14) -0.4814(12) -0.0941(11) 0.090(2) Uiso 0.20 d PD 2
Cl4 Cl 0.3986(23) -0.5032(20) -0.0866(18) 0.086(4) Uiso 0.10 d PD 3
Cl5 Cl 0.3643(12) -0.2894(12) -0.0550(11) 0.112(3) Uiso 0.25 d PD 4
Cl6 Cl 0.5462(9) -0.4703(9) -0.1375(10) 0.090(2) Uiso 0.25 d PD 4
C19 C 0.4010(12) -0.4245(10) -0.1895(10) 0.141(4) Uani 1 d D .
Mo Mo 0.16247(3) 0.18294(3) 0.43041(3) 0.0339(2) Uani 1 d . .
O1 O 0.3671(3) 0.3094(3) 0.4556(3) 0.0369(6) Uani 1 d . .
O2 O 0.0916(3) 0.3379(3) 0.4208(3) 0.0422(6) Uani 1 d . .
O3 O 0.2062(3) 0.1897(3) 0.6057(3) 0.0457(7) Uani 1 d . .
O4 O 0.1253(4) 0.2895(4) 0.6182(3) 0.0507(7) Uani 1 d . .
O5 O 0.0201(3) 0.0299(4) 0.3546(3) 0.0485(7) Uani 1 d . .
N1 N 0.2912(3) 0.0281(3) 0.3708(3) 0.0342(7) Uani 1 d . .
N2 N 0.1786(3) 0.1437(4) 0.2098(3) 0.0366(7) Uani 1 d . .
C1 C 0.2441(5) -0.1176(5) 0.3248(5) 0.0473(10) Uani 1 d . .
H1 H 0.1471 -0.1621 0.3181 0.059 Uiso 1 calc . .
C2 C 0.3370(6) -0.2054(5) 0.2863(5) 0.0531(11) Uani 1 d . .
H2 H 0.3013 -0.3074 0.2520 0.042 Uiso 1 calc . .
C3 C 0.4804(6) -0.1409(5) 0.2992(5) 0.0509(11) Uani 1 d . .
H3 H 0.5425 -0.1990 0.2749 0.066 Uiso 1 calc . .
C4 C 0.5342(5) 0.0129(5) 0.3490(4) 0.0399(9) Uani 1 d . .
C5 C 0.6801(5) 0.0946(6) 0.3701(5) 0.0495(11) Uani 1 d . .
H5 H 0.7503 0.0463 0.3504 0.053 Uiso 1 calc . .
C6 C 0.7163(4) 0.2425(6) 0.4188(5) 0.0524(11) Uani 1 d . .
H6 H 0.8125 0.2941 0.4324 0.079 Uiso 1 calc . .
C7 C 0.6157(4) 0.3234(5) 0.4502(5) 0.0438(9) Uani 1 d . .
H7 H 0.6453 0.4254 0.4832 0.052 Uiso 1 calc . .
C8 C 0.4734(4) 0.2489(4) 0.4314(4) 0.0338(8) Uani 1 d . .
C9 C 0.4339(4) 0.0932(4) 0.3824(4) 0.0333(8) Uani 1 d . .
C10 C 0.2228(5) 0.0422(5) 0.1042(5) 0.0480(10) Uani 1 d . .
H10 H 0.2583 -0.0234 0.1189 0.038 Uiso 1 calc . .
C11 C 0.2176(6) 0.0313(6) -0.0284(5) 0.0558(11) Uani 1 d . .
H11 H 0.2486 -0.0413 -0.1000 0.082 Uiso 1 calc . .
C12 C 0.1674(5) 0.1264(6) -0.0522(5) 0.0545(12) Uani 1 d . .
H12 H 0.1655 0.1206 -0.1395 0.105 Uiso 1 calc . .
C13 C 0.1185(5) 0.2331(5) 0.0556(5) 0.0470(10) Uani 1 d . .
C14 C 0.0605(6) 0.3344(7) 0.0422(6) 0.0614(13) Uani 1 d . .
H14 H 0.0557 0.3355 -0.0420 0.044 Uiso 1 calc . .
C15 C 0.0112(6) 0.4311(7) 0.1525(6) 0.0639(14) Uani 1 d . .
H15 H -0.0298 0.4951 0.1409 0.061 Uiso 1 calc . .
C16 C 0.0205(5) 0.4372(6) 0.2850(6) 0.0541(11) Uani 1 d . .
H16 H -0.0121 0.5053 0.3595 0.084 Uiso 1 calc . .
C17 C 0.0787(4) 0.3403(5) 0.2997(4) 0.0394(9) Uani 1 d . .
C18 C 0.1265(4) 0.2379(5) 0.1861(4) 0.0389(8) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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_3
C19 Cl3 Cl3 151.5(11) 2_645
Cl2 C19 Cl1 116.3(6) .
Cl5 C19 Cl6 110.0(7) .
O5 Mo O4 104.1(2) .
O5 Mo O3 100.83(15) .
O4 Mo O3 43.86(13) .
O5 Mo O2 103.30(14) .
O4 Mo O2 78.77(12) .
O3 Mo O2 121.61(13) .
O5 Mo O1 156.25(14) .
O4 Mo O1 97.93(13) .
O3 Mo O1 88.90(12) .
O2 Mo O1 89.46(11) .
O5 Mo N1 85.71(13) .
O4 Mo N1 122.75(12) .
O3 Mo N1 78.93(12) .
O2 Mo N1 154.41(12) .
O1 Mo N1 74.87(11) .
O5 Mo N2 84.23(14) .
O4 Mo N2 154.03(13) .
O3 Mo N2 159.72(13) .
O2 Mo N2 75.36(12) .
O1 Mo N2 79.69(11) .
N1 Mo N2 81.91(12) .
C8 O1 Mo 120.3(2) .
C17 O2 Mo 120.1(2) .
O4 O3 Mo 67.8(2) .
O3 O4 Mo 68.3(2) .
C1 N1 C9 119.0(4) .
C1 N1 Mo 127.0(3) .
C9 N1 Mo 114.0(2) .
C10 N2 C18 118.1(4) .
C10 N2 Mo 130.7(3) .
C18 N2 Mo 111.1(3) .
N1 C1 C2 121.6(4) .
N1 C1 H1 119.2(4) .
C2 C1 H1 119.2(4) .
C3 C2 C1 119.9(4) .
C3 C2 H2 120.1(5) .
C1 C2 H2 120.1(5) .
C2 C3 C4 120.1(4) .
C2 C3 H3 119.9(5) .
C4 C3 H3 119.9(5) .
C3 C4 C9 116.7(4) .
C3 C4 C5 126.1(4) .
C9 C4 C5 117.1(4) .
C6 C5 C4 119.6(4) .
C6 C5 H5 120.2(5) .
C4 C5 H5 120.2(5) .
C5 C6 C7 123.4(4) .
C5 C6 H6 118.3(5) .
C7 C6 H6 118.3(5) .
C8 C7 C6 118.9(4) .
C8 C7 H7 120.5(4) .
C6 C7 H7 120.5(4) .
O1 C8 C7 125.7(4) .
O1 C8 C9 116.0(3) .
C7 C8 C9 118.3(4) .
N1 C9 C4 122.7(4) .
N1 C9 C8 114.7(3) .
C4 C9 C8 122.6(4) .
N2 C10 C11 122.1(4) .
N2 C10 H10 119.0(4) .
C11 C10 H10 119.0(4) .
C12 C11 C10 120.1(4) .
C12 C11 H11 120.0(5) .
C10 C11 H11 120.0(5) .
C11 C12 C13 119.4(4) .
C11 C12 H12 120.3(5) .
C13 C12 H12 120.3(5) .
C12 C13 C18 117.6(4) .
C12 C13 C14 124.5(4) .
C18 C13 C14 117.9(4) .
C15 C14 C13 120.1(4) .
C15 C14 H14 120.0(5) .
C13 C14 H14 120.0(6) .
C14 C15 C16 122.1(4) .
C14 C15 H15 118.9(6) .
C16 C15 H15 118.9(6) .
C17 C16 C15 118.2(5) .
C17 C16 H16 120.9(5) .
C15 C16 H16 120.9(5) .
O2 C17 C16 122.4(4) .
O2 C17 C18 117.5(3) .
C16 C17 C18 120.1(4) .
N2 C18 C17 115.8(4) .
N2 C18 C13 122.7(4) .
C17 C18 C13 121.5(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 C19 1.767(9) .
Cl2 C19 1.536(10) .
Cl3 C19 1.735(12) .
Cl3 Cl3 2.30(2) 2_645
Cl4 C19 1.69(2) .
Cl5 C19 1.634(13) .
Cl6 C19 1.788(11) .
Mo O5 1.685(3) .
Mo O4 1.925(3) .
Mo O3 1.933(3) .
Mo O2 1.993(3) .
Mo O1 2.037(3) .
Mo N1 2.194(3) .
Mo N2 2.269(3) .
O1 C8 1.327(5) .
O2 C17 1.345(5) .
O3 O4 1.441(4) .
N1 C1 1.331(5) .
N1 C9 1.365(5) .
N2 C10 1.333(5) .
N2 C18 1.357(5) .
C1 C2 1.399(7) .
C1 H1 0.930(5) .
C2 C3 1.368(8) .
C2 H2 0.930(4) .
C3 C4 1.405(6) .
C3 H3 0.930(4) .
C4 C9 1.406(5) .
C4 C5 1.420(7) .
C5 C6 1.348(8) .
C5 H5 0.930(4) .
C6 C7 1.413(7) .
C6 H6 0.930(4) .
C7 C8 1.372(6) .
C7 H7 0.930(4) .
C8 C9 1.422(5) .
C10 C11 1.403(7) .
C10 H10 0.930(5) .
C11 C12 1.356(8) .
C11 H11 0.930(5) .
C12 C13 1.398(7) .
C12 H12 0.930(5) .
C13 C18 1.409(6) .
C13 C14 1.404(7) .
C14 C15 1.363(8) .
C14 H14 0.930(5) .
C15 C16 1.425(7) .
C15 H15 0.930(5) .
C16 C17 1.369(6) .
C16 H16 0.930(5) .
C17 C18 1.402(6) .
