#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322337.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_4322337
loop_
_publ_author_name
'F. Albert Cotton'
'Evgeny V. Dikarev'
'Santiago Herrero'
'Barbara Modec'
_publ_section_title
;
 Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 4. Rotational
 Isomers of Mo2Cl4(R-py)4 (R-py = 4-Picoline, 3,5-Lutidine, and
 4-tert-Butylpyridine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4882
_journal_page_last               4887
_journal_paper_doi               10.1021/ic990728k
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Mo2 Cl4 (N C5 H4 C H3)4'
_chemical_formula_structural     '1,3,6,8 (D2d)-Mo2Cl4(4-pic)4'
_chemical_formula_sum            'C24 H28 Cl4 Mo2 N4'
_chemical_formula_weight         706.18
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Bis(trans-dichloro-bis(4-methylpyridine))-di-molybdenum (II),
 D2d-isomer
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                91.90(1)
_cell_angle_beta                 104.25(2)
_cell_angle_gamma                110.458(8)
_cell_formula_units_Z            2
_cell_length_a                   9.2958(3)
_cell_length_b                   10.2669(7)
_cell_length_c                   16.254(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.0
_cell_volume                     1396.5(3)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7704
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_obs          0.0463
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0717P)²+6.5763P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1337
_refine_ls_wR_factor_obs         0.1237
_reflns_number_observed          3072
_reflns_number_total             3506
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990728k_3.cif
_cod_data_source_block           Mo2Cl4(4-pic)4_(1b)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+6.5763P] 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^)+(0.0717P)^2^+6.5763P] 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               4322337
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
Mo1 Mo 0.70537(6) 0.02488(6) 0.82944(3) 0.0202(2) Uani 1 d . .
Mo2 Mo 0.61600(6) -0.06198(6) 0.69657(3) 0.0212(2) Uani 1 d . .
Cl1 Cl 0.5260(2) -0.1249(2) 0.90249(11) 0.0292(4) Uani 1 d . .
Cl2 Cl 0.9410(2) 0.2321(2) 0.84338(12) 0.0311(4) Uani 1 d . .
Cl3 Cl 0.7034(2) -0.2543(2) 0.67985(12) 0.0332(4) Uani 1 d . .
Cl4 Cl 0.4648(2) 0.0685(2) 0.62444(11) 0.0327(4) Uani 1 d . .
N1 N 0.8585(6) -0.1005(6) 0.8769(3) 0.0246(13) Uani 1 d . .
N2 N 0.5818(6) 0.1773(6) 0.8322(3) 0.0232(13) Uani 1 d . .
N3 N 0.3751(7) -0.2210(6) 0.6897(4) 0.0265(13) Uani 1 d . .
N4 N 0.8179(7) 0.0592(6) 0.6439(4) 0.0263(13) Uani 1 d . .
C1 C 0.7928(8) -0.2385(7) 0.8789(4) 0.029(2) Uani 1 d . .
H1 H 0.6808(8) -0.2810(7) 0.8622(4) 0.035 Uiso 1 calc R .
C2 C 0.8799(9) -0.3219(8) 0.9041(5) 0.035(2) Uani 1 d . .
H2 H 0.8271(9) -0.4183(8) 0.9048(5) 0.042 Uiso 1 calc R .
C3 C 1.0449(8) -0.2638(8) 0.9281(4) 0.027(2) Uani 1 d . .
C4 C 1.1133(8) -0.1208(7) 0.9265(5) 0.031(2) Uani 1 d . .
H4 H 1.2251(8) -0.0762(7) 0.9428(5) 0.038 Uiso 1 calc R .
C5 C 1.0199(8) -0.0432(7) 0.9013(4) 0.026(2) Uani 1 d . .
H5 H 1.0702(8) 0.0537(7) 0.9010(4) 0.032 Uiso 1 calc R .
C6 C 1.1432(9) -0.3522(8) 0.9536(5) 0.039(2) Uani 1 d . .
H6A H 1.1633(54) -0.3567(46) 1.0147(8) 0.059 Uiso 1 calc R .
H6B H 1.2440(28) -0.3111(31) 0.9397(32) 0.059 Uiso 1 calc R .
H6C H 1.0859(29) -0.4461(17) 0.9228(26) 0.059 Uiso 1 calc R .
C7 C 0.6062(8) 0.2854(7) 0.7864(5) 0.030(2) Uani 1 d . .
H7 H 0.6743(8) 0.2949(7) 0.7508(5) 0.036 Uiso 1 calc R .
C8 C 0.5359(9) 0.3836(8) 0.7889(5) 0.035(2) Uani 1 d . .
H8 H 0.5560(9) 0.4564(8) 0.7547(5) 0.042 Uiso 1 calc R .
C9 C 0.4384(9) 0.3762(8) 0.8400(6) 0.039(2) Uani 1 d . .
C10 C 0.4150(9) 0.2667(8) 0.8890(5) 0.038(2) Uani 1 d . .
H10 H 0.3503(9) 0.2580(8) 0.9264(5) 0.046 Uiso 1 calc R .
C11 C 0.4863(8) 0.1699(7) 0.8832(5) 0.030(2) Uani 1 d . .
H11 H 0.4670(8) 0.0958(7) 0.9165(5) 0.036 Uiso 1 calc R .
C12 C 0.3572(11) 0.4790(9) 0.8464(8) 0.061(3) Uani 1 d . .
H12A H 0.3962(64) 0.5284(54) 0.9041(14) 0.092 Uiso 1 calc R .
H12B H 0.2427(13) 0.4287(12) 0.8329(46) 0.092 Uiso 1 calc R .
H12C H 0.3805(71) 0.5458(47) 0.8061(33) 0.092 Uiso 1 calc R .
C13 C 0.2680(9) -0.1847(8) 0.7197(5) 0.032(2) Uani 1 d . .
H13 H 0.3010(9) -0.0943(8) 0.7490(5) 0.038 Uiso 1 calc R .
C14 C 0.1127(8) -0.2754(8) 0.7086(5) 0.032(2) Uani 1 d . .
H14 H 0.0432(8) -0.2456(8) 0.7306(5) 0.039 Uiso 1 calc R .
C15 C 0.0581(9) -0.4089(8) 0.6660(6) 0.040(2) Uani 1 d . .
C16 C 0.1654(9) -0.4421(8) 0.6316(6) 0.050(2) Uani 1 d . .
H16 H 0.1325(9) -0.5296(8) 0.5986(6) 0.061 Uiso 1 calc R .
C17 C 0.3194(9) -0.3485(8) 0.6451(5) 0.040(2) Uani 1 d . .
H17 H 0.3892(9) -0.3757(8) 0.6218(5) 0.048 Uiso 1 calc R .
C18 C -0.1069(11) -0.5129(10) 0.6573(8) 0.064(3) Uani 1 d . .
H18A H -0.1001(11) -0.5897(40) 0.6892(39) 0.096 Uiso 1 calc R .
H18B H -0.1599(33) -0.5489(57) 0.5973(9) 0.096 Uiso 1 calc R .
H18C H -0.1674(30) -0.4673(22) 0.6796(43) 0.096 Uiso 1 calc R .
C19 C 0.9674(9) 0.0618(8) 0.6793(5) 0.034(2) Uani 1 d . .
H19 H 0.9879(9) 0.0239(8) 0.7308(5) 0.040 Uiso 1 calc R .
C20 C 1.0898(9) 0.1179(8) 0.6423(5) 0.035(2) Uani 1 d . .
H20 H 1.1923(9) 0.1193(8) 0.6690(5) 0.042 Uiso 1 calc R .
C21 C 1.0619(9) 0.1728(7) 0.5652(4) 0.029(2) Uani 1 d . .
C22 C 0.9099(9) 0.1666(8) 0.5314(5) 0.032(2) Uani 1 d . .
H22 H 0.8849(9) 0.2013(8) 0.4792(5) 0.038 Uiso 1 calc R .
C23 C 0.7918(9) 0.1108(7) 0.5716(5) 0.030(2) Uani 1 d . .
H23 H 0.6890(9) 0.1098(7) 0.5461(5) 0.036 Uiso 1 calc R .
C24 C 1.1940(10) 0.2341(9) 0.5239(5) 0.044(2) Uani 1 d . .
H24A H 1.2372(44) 0.1638(20) 0.5132(32) 0.065 Uiso 1 calc R .
H24B H 1.2777(31) 0.3140(36) 0.5617(16) 0.065 Uiso 1 calc R .
H24C H 1.1526(17) 0.2640(52) 0.4702(18) 0.065 Uiso 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'
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
Mo2 Mo1 N2 101.11(14) . . y
Mo2 Mo1 N1 99.31(14) . . y
N2 Mo1 N1 159.5(2) . . y
Mo2 Mo1 Cl2 107.20(5) . . y
N2 Mo1 Cl2 84.66(15) . . y
N1 Mo1 Cl2 90.63(15) . . y
Mo2 Mo1 Cl1 106.67(5) . . y
N2 Mo1 Cl1 88.40(14) . . y
N1 Mo1 Cl1 84.46(15) . . y
Cl2 Mo1 Cl1 146.13(7) . . y
Mo1 Mo2 N3 102.62(15) . . y
Mo1 Mo2 N4 102.12(15) . . y
N3 Mo2 N4 155.3(2) . . y
Mo1 Mo2 Cl4 107.26(5) . . y
N3 Mo2 Cl4 83.64(15) . . y
N4 Mo2 Cl4 89.0(2) . . y
Mo1 Mo2 Cl3 107.72(5) . . y
N3 Mo2 Cl3 87.8(2) . . y
N4 Mo2 Cl3 84.8(2) . . y
Cl4 Mo2 Cl3 145.00(7) . . y
C1 N1 C5 116.3(6) . . n
C1 N1 Mo1 121.0(4) . . n
C5 N1 Mo1 122.6(4) . . n
C11 N2 C7 116.3(6) . . n
C11 N2 Mo1 121.9(5) . . n
C7 N2 Mo1 121.8(4) . . n
C17 N3 C13 116.0(6) . . n
C17 N3 Mo2 122.3(5) . . n
C13 N3 Mo2 120.8(5) . . n
C23 N4 C19 117.7(6) . . n
C23 N4 Mo2 121.3(5) . . n
C19 N4 Mo2 120.2(5) . . n
N1 C1 C2 123.8(7) . . n
C1 C2 C3 119.9(7) . . n
C2 C3 C4 116.4(6) . . n
C2 C3 C6 121.3(7) . . n
C4 C3 C6 122.3(7) . . n
C5 C4 C3 120.9(7) . . n
N1 C5 C4 122.7(6) . . n
N2 C7 C8 123.1(6) . . n
C9 C8 C7 121.0(7) . . n
C8 C9 C10 116.4(7) . . n
C8 C9 C12 124.2(8) . . n
C10 C9 C12 119.4(8) . . n
C9 C10 C11 120.4(7) . . n
N2 C11 C10 122.9(7) . . n
N3 C13 C14 122.6(7) . . n
C15 C14 C13 121.0(7) . . n
C14 C15 C16 115.9(7) . . n
C14 C15 C18 122.4(8) . . n
C16 C15 C18 121.7(8) . . n
C17 C16 C15 120.8(7) . . n
N3 C17 C16 123.5(7) . . n
N4 C19 C20 122.3(7) . . n
C19 C20 C21 120.0(7) . . n
C22 C21 C20 115.8(6) . . n
C22 C21 C24 123.5(7) . . n
C20 C21 C24 120.7(7) . . n
C21 C22 C23 121.9(7) . . n
N4 C23 C22 122.3(7) . . n
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 Mo2 2.1497(9) . y
Mo1 N2 2.247(6) . y
Mo1 N1 2.254(6) . y
Mo1 Cl2 2.417(2) . y
Mo1 Cl1 2.421(2) . y
Mo2 N3 2.237(6) . y
Mo2 N4 2.243(6) . y
Mo2 Cl4 2.398(2) . y
Mo2 Cl3 2.414(2) . y
N1 C1 1.338(9) . n
N1 C5 1.353(9) . n
N2 C11 1.342(9) . n
N2 C7 1.342(9) . n
N3 C17 1.337(9) . n
N3 C13 1.361(9) . n
N4 C23 1.309(9) . n
N4 C19 1.357(9) . n
C1 C2 1.380(10) . n
C2 C3 1.382(10) . n
C3 C4 1.386(10) . n
C3 C6 1.500(10) . n
C4 C5 1.374(10) . n
C7 C8 1.384(10) . n
C8 C9 1.359(11) . n
C9 C10 1.386(11) . n
C9 C12 1.510(11) . n
C10 C11 1.387(10) . n
C13 C14 1.380(10) . n
C14 C15 1.376(11) . n
C15 C16 1.388(12) . n
C15 C18 1.500(11) . n
C16 C17 1.375(11) . n
C19 C20 1.374(11) . n
C20 C21 1.395(11) . n
C21 C22 1.362(10) . n
C21 C24 1.500(10) . n
C22 C23 1.377(10) . n
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
N1 Mo1 Mo2 N3 98.1(2) . . . . n
N1 Mo1 Mo2 N4 -81.9(2) . . . . n
N1 Mo1 Mo2 Cl3 6.37(15) . . . . y
N1 Mo1 Mo2 Cl4 -174.68(14) . . . . n
N2 Mo1 Mo2 N3 -80.5(2) . . . . n
N2 Mo1 Mo2 N4 99.4(2) . . . . n
N2 Mo1 Mo2 Cl3 -172.26(15) . . . . n
N2 Mo1 Mo2 Cl4 6.69(15) . . . . y
Cl1 Mo1 Mo2 N3 11.2(2) . . . . y
Cl1 Mo1 Mo2 N4 -168.9(2) . . . . n
Cl1 Mo1 Mo2 Cl3 -80.60(7) . . . . n
Cl1 Mo1 Mo2 Cl4 98.36(7) . . . . n
Cl2 Mo1 Mo2 N3 -168.3(2) . . . . n
Cl2 Mo1 Mo2 N4 11.6(2) . . . . y
Cl2 Mo1 Mo2 Cl3 99.95(7) . . . . n
Cl2 Mo1 Mo2 Cl4 -81.10(7) . . . . n
Mo2 Mo1 N1 C1 -67.8(5) . . . . n
Mo2 Mo1 N1 C5 109.4(5) . . . . n
Mo2 Mo1 N2 C7 -61.7(5) . . . . n
Mo2 Mo1 N2 C11 122.0(5) . . . . n
Mo1 Mo2 N3 C13 53.0(5) . . . . n
Mo1 Mo2 N3 C17 -137.5(6) . . . . n
Mo1 Mo2 N4 C19 55.1(5) . . . . n
Mo1 Mo2 N4 C23 -135.4(5) . . . . n
