#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/75/4307547.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_4307547
loop_
_publ_author_name
'Farideh Jalilehvand'
'Vicky Mah'
'Bonnie O. Leung'
'Daniel Ross'
'Masood Parvez'
'Ricardo F. Aroca'
_publ_contact_author
;
    Masood Parvez
    Department of Chemistry
    University of Calgary
    2500 University Drive N.W.
    Calgary, Alberta, Canada T2N 1N4  
;
_publ_contact_author_email       ' parvez@ucalgary.ca '
_publ_contact_author_fax         ' (403)289-9488 '
_publ_contact_author_phone       ' (403)220-5348 '
_publ_section_title
;
Structural Characterization of Molybdenum(V) Species in Aqueous HCl
Solutions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4430
_journal_page_last               4445
_journal_paper_doi               10.1021/ic062047c
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C12.5 H18 Cl7 Mo1.5 N2.5 O3'
_chemical_formula_weight         643.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           51
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2a'
_symmetry_space_group_name_H-M   'P m m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.398(3)
_cell_length_b                   8.057(4)
_cell_length_c                   13.330(4)
_cell_measurement_reflns_used    5135
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.9
_cell_volume                     2298.1(14)
_computing_cell_refinement       'HKL DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' ω and φ '
_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  0.031
_diffrn_reflns_av_sigmaI/netI    0.037
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5135
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.9
_exptl_absorpt_coefficient_mu    1.662
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1266
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2888
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.99
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.036
_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)+(0.048P)²+3.30P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.086
_refine_ls_wR_factor_ref         0.098
_reflns_number_gt                2179
_reflns_number_total             2888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062047c-file001.cif
_cod_data_source_block           Compound_I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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_formula_sum        'C12.50 H18 Cl7 Mo1.50 N2.50 O3'
_cod_database_code               4307547
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'x+1/2, -y, -z'
'-x, y, -z'
'-x, -y, -z'
'x-1/2, y, -z'
'-x-1/2, 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_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
Mo1 Mo 0.2500 0.5000 0.27512(4) 0.02885(16) Uani 1 4 d S . .
Mo2 Mo 0.072841(18) 0.5000 0.78072(3) 0.03065(15) Uani 1 2 d S . .
Cl1 Cl 0.2500 0.21054(15) 0.30512(10) 0.0432(3) Uani 1 2 d S . .
Cl2 Cl 0.13960(6) 0.5000 0.29540(15) 0.0645(5) Uani 1 2 d S . .
Cl3 Cl 0.1285(2) 0.5000 0.9387(4) 0.0507(10) Uani 0.881(18) 2 d SP A 1
Cl3' Cl 0.1465(15) 0.5000 0.906(2) 0.0507(10) Uani 0.119(18) 2 d SP A 2
Cl4 Cl 0.04440(7) 0.5000 0.60996(10) 0.0488(3) Uani 1 2 d S A .
Cl5 Cl 0.08920(4) 0.20964(11) 0.76882(7) 0.0466(2) Uani 1 1 d . A .
Cl6 Cl 0.2500 0.22182(14) 0.61344(8) 0.0327(3) Uani 1 2 d S . .
O1 O 0.2500 0.5000 0.1520(4) 0.0546(15) Uani 1 4 d S . .
O2 O 0.2500 0.5000 0.4460(4) 0.0609(17) Uani 1 4 d SD . .
H02 H 0.2500 0.4190 0.4830 0.073 Uiso 1 2 d SD . .
O3 O 0.00291(18) 0.5000 0.8319(3) 0.0612(11) Uani 1 2 d S A .
O4 O 0.17159(17) 0.5000 0.7188(3) 0.0493(10) Uani 1 2 d SD A .
H04 H 0.1851 0.4250 0.6830 0.059 Uiso 1 1 d D . .
N1 N 0.13736(19) 0.0000 0.5061(3) 0.0422(10) Uani 1 2 d S . .
H1 H 0.1709 0.0000 0.5443 0.051 Uiso 1 2 calc SR . .
C1 C 0.11368(17) 0.1444(5) 0.4792(3) 0.0455(9) Uani 1 1 d . . .
H1A H 0.1327 0.2448 0.5005 0.055 Uiso 1 1 calc R . .
C2 C 0.06161(17) 0.1481(5) 0.4203(3) 0.0457(9) Uani 1 1 d . . .
H2A H 0.0437 0.2509 0.4005 0.055 Uiso 1 1 calc R . .
C3 C 0.0355(2) 0.0000 0.3903(4) 0.0462(14) Uani 1 2 d S . .
H3A H -0.0006 0.0000 0.3488 0.055 Uiso 1 2 calc SR . .
N2 N 0.2500 0.0000 0.8284(5) 0.0522(18) Uani 1 4 d S . .
H2 H 0.2500 0.0000 0.7624 0.063 Uiso 1 4 calc SR . .
C4 C 0.2500 0.1437(9) 0.8752(5) 0.0592(17) Uani 1 2 d S . .
H4 H 0.2500 0.2442 0.8380 0.071 Uiso 1 2 calc SR . .
C5 C 0.2500 0.1477(7) 0.9782(4) 0.0479(14) Uani 1 2 d S . .
H5 H 0.2500 0.2505 1.0131 0.058 Uiso 1 2 calc SR . .
C6 C 0.2500 0.0000 1.0298(5) 0.0402(17) Uani 1 4 d S . .
H6 H 0.2500 0.0000 1.1010 0.048 Uiso 1 4 calc SR . .
N3 N 0.5787(4) 0.0000 -0.0017(6) 0.136(4) Uani 1 2 d S . .
H3 H 0.5670 0.0000 0.0616 0.163 Uiso 1 2 calc SR . .
C7 C 0.5873(3) -0.1395(8) -0.0482(8) 0.111(3) Uani 1 1 d . . .
H7 H 0.5787 -0.2413 -0.0149 0.134 Uiso 1 1 calc R . .
C8 C 0.6070(3) -0.1408(11) -0.1374(8) 0.130(4) Uani 1 1 d . . .
H8 H 0.6130 -0.2435 -0.1711 0.156 Uiso 1 1 calc R . .
C9 C 0.6194(4) 0.0000 -0.1841(5) 0.150(7) Uani 1 2 d S . .
H9 H 0.6368 0.0000 -0.2497 0.180 Uiso 1 2 calc SR . .
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'
Cl Cl 0.1484 0.1585 '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
O1 Mo1 O2 180.000(1) . . ?
O1 Mo1 Cl1 99.73(4) . 2_565 ?
O2 Mo1 Cl1 80.27(4) . 2_565 ?
O1 Mo1 Cl1 99.73(4) . . ?
O2 Mo1 Cl1 80.27(4) . . ?
Cl1 Mo1 Cl1 160.54(7) 2_565 . ?
O1 Mo1 Cl2 96.53(5) . 2_565 ?
O2 Mo1 Cl2 83.47(5) . 2_565 ?
Cl1 Mo1 Cl2 88.899(10) 2_565 2_565 ?
Cl1 Mo1 Cl2 88.899(10) . 2_565 ?
O1 Mo1 Cl2 96.53(5) . . ?
O2 Mo1 Cl2 83.47(5) . . ?
Cl1 Mo1 Cl2 88.899(10) 2_565 . ?
Cl1 Mo1 Cl2 88.899(10) . . ?
Cl2 Mo1 Cl2 166.95(10) 2_565 . ?
O3 Mo2 O4 176.8(2) . . ?
O3 Mo2 Cl3' 108.8(10) . . ?
O4 Mo2 Cl3' 68.0(10) . . ?
O3 Mo2 Cl4 99.54(17) . . ?
O4 Mo2 Cl4 83.62(13) . . ?
Cl3' Mo2 Cl4 151.6(10) . . ?
O3 Mo2 Cl5 99.33(3) . 8_565 ?
O4 Mo2 Cl5 80.68(3) . 8_565 ?
Cl3' Mo2 Cl5 86.98(16) . 8_565 ?
Cl4 Mo2 Cl5 88.48(3) . 8_565 ?
O3 Mo2 Cl5 99.33(3) . . ?
O4 Mo2 Cl5 80.68(3) . . ?
Cl3' Mo2 Cl5 86.98(16) . . ?
Cl4 Mo2 Cl5 88.48(3) . . ?
Cl5 Mo2 Cl5 161.34(5) 8_565 . ?
O3 Mo2 Cl3 95.0(2) . . ?
O4 Mo2 Cl3 81.9(2) . . ?
Cl3' Mo2 Cl3 13.9(9) . . ?
Cl4 Mo2 Cl3 165.49(17) . . ?
Cl5 Mo2 Cl3 89.17(4) 8_565 . ?
Cl5 Mo2 Cl3 89.17(4) . . ?
Mo1 O2 H02 128 . . ?
Mo2 O4 H04 123 . . ?
C1 N1 C1 123.8(4) 8 . ?
C1 N1 H1 118.1 8 . ?
C1 N1 H1 118.1 . . ?
N1 C1 C2 119.4(4) . . ?
N1 C1 H1A 120.3 . . ?
C2 C1 H1A 120.3 . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 H2A 120.6 . . ?
C1 C2 H2A 120.6 . . ?
C2 C3 C2 120.1(5) . 8 ?
C2 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 8 . ?
C4 N2 C4 123.4(7) . 2 ?
C4 N2 H2 118.3 . . ?
C4 N2 H2 118.3 2 . ?
N2 C4 C5 119.7(6) . . ?
N2 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 118.7(6) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
C5 C6 C5 120.0(7) . 2 ?
C5 C6 H6 120.0 . . ?
C5 C6 H6 120.0 2 . ?
C7 N3 C7 120.2(9) 8 . ?
C7 N3 H3 119.9 8 . ?
C7 N3 H3 119.9 . . ?
N3 C7 C8 120.3(7) . . ?
N3 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 120.3(7) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C8 118.4(8) 8 . ?
C8 C9 H9 120.8 8 . ?
C8 C9 H9 120.8 . . ?
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
Mo1 O1 1.641(5) . ?
Mo1 O2 2.278(5) . ?
Mo1 Cl1 2.3662(17) 2_565 ?
Mo1 Cl1 2.3662(17) . ?
Mo1 Cl2 2.3777(14) 2_565 ?
Mo1 Cl2 2.3777(14) . ?
Mo2 O3 1.645(4) . ?
Mo2 O4 2.269(4) . ?
Mo2 Cl3' 2.297(19) . ?
Mo2 Cl4 2.3562(15) . ?
Mo2 Cl5 2.3708(15) 8_565 ?
Mo2 Cl5 2.3708(15) . ?
Mo2 Cl3 2.419(3) . ?
O2 H02 0.8200 . ?
O4 H04 0.8200 . ?
N1 C1 1.319(4) 8 ?
N1 C1 1.319(4) . ?
N1 H1 0.8800 . ?
C1 C2 1.363(5) . ?
C1 H1A 0.9500 . ?
C2 C3 1.378(5) . ?
C2 H2A 0.9500 . ?
C3 C2 1.378(5) 8 ?
C3 H3A 0.9500 . ?
N2 C4 1.315(8) . ?
N2 C4 1.315(8) 2 ?
N2 H2 0.8800 . ?
C4 C5 1.373(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.374(7) . ?
C5 H5 0.9500 . ?
C6 C5 1.374(7) 2 ?
C6 H6 0.9500 . ?
N3 C7 1.297(9) 8 ?
N3 C7 1.297(9) . ?
N3 H3 0.8800 . ?
C7 C8 1.261(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.321(11) . ?
C8 H8 0.9500 . ?
C9 C8 1.321(11) 8 ?
C9 H9 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H02 Cl6 0.82 2.35 3.163(4) 170 .
O4 H04 Cl6 0.82 2.34 3.132(3) 162 .
N1 H1 Cl6 0.88 2.63 3.324(4) 137 .
N1 H1 Cl6 0.88 2.63 3.324(4) 137 2
N2 H2 Cl6 0.88 2.67 3.378(6) 138 2
N2 H2 Cl6 0.88 2.67 3.378(6) 138 .
N3 H3 Cl5 0.88 2.86 3.541(7) 135 6_656
N3 H3 Cl5 0.88 2.86 3.541(7) 135 3_556
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C1 C2 0.2(8) 8 . . . ?
N1 C1 C2 C3 -0.4(6) . . . . ?
C1 C2 C3 C2 0.5(7) . . . 8 ?
C4 N2 C4 C5 0.000(3) 2 . . . ?
N2 C4 C5 C6 0.000(3) . . . . ?
C4 C5 C6 C5 0.000(3) . . . 2 ?
C7 N3 C7 C8 3.5(16) 8 . . . ?
N3 C7 C8 C9 0.4(13) . . . . ?
C7 C8 C9 C8 -4.1(15) . . . 8 ?
