#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:53:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179941 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/36/7023696.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_7023696
loop_
_publ_author_name
'Marchetti, Fabio'
'Pampaloni, Guido'
'Zacchini, Stefano'
_publ_section_title
;
 The reactivity of molybdenum pentachloride with ethers: routes to the
 synthesis of Mo(IV)Cl4 adducts, Mo(v) chlorido-alkoxides and Mo(v)
 oxydo-chlorides.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15226
_journal_page_last               15234
_journal_paper_doi               10.1039/c3dt51797g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C5 H12 Cl4 Mo O2'
_chemical_formula_weight         341.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n 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                   11.1285(8)
_cell_length_b                   8.9787(7)
_cell_length_c                   11.7001(9)
_cell_measurement_reflns_used    3739
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.615
_cell_measurement_theta_min      2.526
_cell_volume                     1169.07(15)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11125
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.999
_exptl_absorpt_correction_T_max  0.8251
_exptl_absorpt_correction_T_min  0.7404
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.0868 (selected reflections only, before parameter refinement)
 R(int) =  0.0420 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            bright-orange
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.931
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1120
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0954
_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)+(0.0000P)²+48.6585P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2055
_reflns_number_gt                1007
_reflns_number_total             1120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51797g.txt
_cod_data_source_block           pnma
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7023696
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Mo1 Mo 0.73615(14) 0.2500 0.50415(14) 0.0327(5) Uani 1 2 d S . .
Cl1 Cl 0.6303(6) 0.2500 0.6728(5) 0.090(3) Uani 1 2 d SU A .
Cl2 Cl 0.8344(5) 0.2500 0.3275(4) 0.0410(12) Uani 1 2 d SU A .
Cl3 Cl 0.6137(15) 0.4402(16) 0.4474(11) 0.054(3) Uani 0.50 1 d PU A -1
Cl4 Cl 0.8755(9) 0.3955(12) 0.5837(8) 0.065(2) Uani 0.50 1 d PU A -1
C1 C 0.898(3) 0.026(4) 0.651(2) 0.049(7) Uani 0.50 1 d PDU A -1
H1A H 0.9385 0.1205 0.6666 0.073 Uiso 0.50 1 calc PR A -1
H1B H 0.9580 -0.0532 0.6420 0.073 Uiso 0.50 1 calc PR A -1
H1C H 0.8449 0.0010 0.7154 0.073 Uiso 0.50 1 calc PR A -1
O1 O 0.8281(17) 0.038(2) 0.5485(16) 0.042(4) Uani 0.50 1 d PDU A -1
C2 C 0.753(2) -0.087(2) 0.528(2) 0.053(5) Uani 0.50 1 d PDU A -1
H2 H 0.6963 -0.1032 0.5929 0.063 Uiso 0.50 1 calc PR A -1
C3 C 0.830(3) -0.226(4) 0.508(3) 0.066(8) Uani 0.50 1 d PDU A -1
H3A H 0.8820 -0.2421 0.5742 0.099 Uiso 0.50 1 calc PR A -1
H3B H 0.8790 -0.2123 0.4393 0.099 Uiso 0.50 1 calc PR A -1
H3C H 0.7773 -0.3129 0.4977 0.099 Uiso 0.50 1 calc PR A -1
C4 C 0.683(3) -0.060(4) 0.417(2) 0.051(5) Uani 0.50 1 d PDU A -1
H4A H 0.7384 -0.0559 0.3510 0.062 Uiso 0.50 1 calc PR A -1
H4B H 0.6247 -0.1422 0.4038 0.062 Uiso 0.50 1 calc PR A -1
O2 O 0.621(4) 0.078(4) 0.430(3) 0.054(7) Uani 0.50 1 d PDU A -1
C5 C 0.545(3) 0.119(4) 0.336(3) 0.057(7) Uani 0.50 1 d PDU A -1
H5A H 0.4997 0.2093 0.3563 0.086 Uiso 0.50 1 calc PR A -1
H5B H 0.4889 0.0381 0.3194 0.086 Uiso 0.50 1 calc PR A -1
H5C H 0.5944 0.1394 0.2684 0.086 Uiso 0.50 1 calc PR A -1
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'
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
O2 Mo1 O2 89.8(14) . 7_565
O2 Mo1 O1 165.3(9) . 7_565
O2 Mo1 O1 76.1(9) 7_565 7_565
O2 Mo1 O1 76.1(9) . .
O2 Mo1 O1 165.3(9) 7_565 .
O1 Mo1 O1 117.8(10) 7_565 .
O2 Mo1 Cl4 170.6(8) . .
O2 Mo1 Cl4 99.2(8) 7_565 .
O1 Mo1 Cl4 23.2(5) 7_565 .
O1 Mo1 Cl4 94.8(6) . .
O2 Mo1 Cl4 99.2(8) . 7_565
O2 Mo1 Cl4 170.6(8) 7_565 7_565
O1 Mo1 Cl4 94.8(6) 7_565 7_565
O1 Mo1 Cl4 23.2(5) . 7_565
Cl4 Mo1 Cl4 71.7(6) . 7_565
O2 Mo1 Cl3 6.7(14) . 7_565
O2 Mo1 Cl3 93.6(6) 7_565 7_565
O1 Mo1 Cl3 169.5(6) 7_565 7_565
O1 Mo1 Cl3 72.7(6) . 7_565
Cl4 Mo1 Cl3 166.9(4) . 7_565
Cl4 Mo1 Cl3 95.7(4) 7_565 7_565
O2 Mo1 Cl3 93.6(6) . .
O2 Mo1 Cl3 6.7(14) 7_565 .
O1 Mo1 Cl3 72.7(6) 7_565 .
O1 Mo1 Cl3 169.5(6) . .
Cl4 Mo1 Cl3 95.7(4) . .
Cl4 Mo1 Cl3 166.9(4) 7_565 .
Cl3 Mo1 Cl3 96.8(7) 7_565 .
O2 Mo1 Cl1 92.4(12) . .
O2 Mo1 Cl1 92.4(12) 7_565 .
O1 Mo1 Cl1 92.0(5) 7_565 .
O1 Mo1 Cl1 92.0(5) . .
Cl4 Mo1 Cl1 89.9(3) . .
Cl4 Mo1 Cl1 89.9(3) 7_565 .
Cl3 Mo1 Cl1 86.8(4) 7_565 .
Cl3 Mo1 Cl1 86.8(4) . .
O2 Mo1 Cl2 85.5(12) . .
O2 Mo1 Cl2 85.5(12) 7_565 .
O1 Mo1 Cl2 89.5(5) 7_565 .
O1 Mo1 Cl2 89.5(5) . .
Cl4 Mo1 Cl2 92.5(3) . .
Cl4 Mo1 Cl2 92.5(3) 7_565 .
Cl3 Mo1 Cl2 91.3(4) 7_565 .
Cl3 Mo1 Cl2 91.3(4) . .
Cl1 Mo1 Cl2 177.0(2) . .
O1 C1 H1A 109.5 . .
O1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
O1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C2 O1 C1 113(2) . .
C2 O1 Mo1 111.5(14) . .
C1 O1 Mo1 120.9(19) . .
O1 C2 C3 110(2) . .
O1 C2 C4 109(2) . .
C3 C2 C4 107(2) . .
O1 C2 H2 110.5 . .
C3 C2 H2 110.5 . .
C4 C2 H2 110.5 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
O2 C4 C2 107(2) . .
O2 C4 H4A 110.3 . .
C2 C4 H4A 110.3 . .
O2 C4 H4B 110.3 . .
C2 C4 H4B 110.3 . .
H4A C4 H4B 108.5 . .
C4 O2 C5 116(3) . .
C4 O2 Mo1 112(3) . .
C5 O2 Mo1 118(3) . .
O2 C5 H5A 109.5 . .
O2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
O2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O2 2.19(5) .
Mo1 O2 2.19(5) 7_565
Mo1 O1 2.22(2) 7_565
Mo1 O1 2.22(2) .
Mo1 Cl4 2.231(10) .
Mo1 Cl4 2.231(10) 7_565
Mo1 Cl3 2.283(16) 7_565
Mo1 Cl3 2.283(16) .
Mo1 Cl1 2.299(6) .
Mo1 Cl2 2.339(5) .
C1 O1 1.437(10) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
O1 C2 1.427(10) .
C2 C3 1.529(10) .
C2 C4 1.530(10) .
C2 H2 1.0000 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 O2 1.428(10) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
O2 C5 1.432(10) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
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
O2 Mo1 O1 C2 -12(2) .
O2 Mo1 O1 C2 -28(6) 7_565
O1 Mo1 O1 C2 173.1(13) 7_565
Cl4 Mo1 O1 C2 169.7(17) .
Cl4 Mo1 O1 C2 165(3) 7_565
Cl3 Mo1 O1 C2 -6.3(16) 7_565
Cl3 Mo1 O1 C2 -4(5) .
Cl1 Mo1 O1 C2 79.7(17) .
Cl2 Mo1 O1 C2 -97.8(17) .
O2 Mo1 O1 C1 -150(2) .
O2 Mo1 O1 C1 -165(5) 7_565
O1 Mo1 O1 C1 36(2) 7_565
Cl4 Mo1 O1 C1 32(2) .
Cl4 Mo1 O1 C1 27.4(18) 7_565
Cl3 Mo1 O1 C1 -144(2) 7_565
Cl3 Mo1 O1 C1 -141(3) .
Cl1 Mo1 O1 C1 -58(2) .
Cl2 Mo1 O1 C1 125(2) .
C1 O1 C2 C3 -64(3) .
Mo1 O1 C2 C3 155.5(18) .
C1 O1 C2 C4 180(2) .
Mo1 O1 C2 C4 39(3) .
O1 C2 C4 O2 -55(4) .
C3 C2 C4 O2 -174(3) .
C2 C4 O2 C5 -177(3) .
C2 C4 O2 Mo1 44(3) .
O2 Mo1 O2 C4 157.4(18) 7_565
O1 Mo1 O2 C4 142(3) 7_565
O1 Mo1 O2 C4 -19(3) .
Cl4 Mo1 O2 C4 -6(10) .
Cl4 Mo1 O2 C4 -20(3) 7_565
Cl3 Mo1 O2 C4 -78(9) 7_565
Cl3 Mo1 O2 C4 163(3) .
Cl1 Mo1 O2 C4 -110(3) .
Cl2 Mo1 O2 C4 72(3) .
O2 Mo1 O2 C5 20(4) 7_565
O1 Mo1 O2 C5 5(8) 7_565
O1 Mo1 O2 C5 -156(3) .
Cl4 Mo1 O2 C5 -144(5) .
Cl4 Mo1 O2 C5 -158(3) 7_565
Cl3 Mo1 O2 C5 144(13) 7_565
Cl3 Mo1 O2 C5 25(3) .
Cl1 Mo1 O2 C5 112(3) .
Cl2 Mo1 O2 C5 -66(3) .
