#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/11/2011150.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2011150
loop_
_publ_author_name
'Modec, Barbara'
'Brenčič, Jurij V.'
'Golič, Ljubo'
_publ_section_title
;
 A 4-ethylpyridine complex of tetrachloromolybdenum(III) and its
 oxidation product
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              780
_journal_page_last               782
_journal_paper_doi               10.1107/S0108270100004911
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Mo Cl4 (C7 H9 N)2]'
_chemical_formula_moiety         'C14 H18 Cl4 Mo1 N2'
_chemical_formula_structural     'Mo Cl4 (C7H9N))2'
_chemical_formula_sum            'C14 H18 Cl4 Mo N2'
_chemical_formula_weight         452.06
_chemical_name_systematic
;
trans-tetrachlorodi(4-ethylpyridine)molybdenum(IV)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 98.012(4)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   16.1077(8)
_cell_length_b                   7.6691(4)
_cell_length_c                   7.1566(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293
_cell_measurement_theta_max      20.10
_cell_measurement_theta_min      10.04
_cell_volume                     875.44(8)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'Xtal3.4 DIFDAT, SORTRF and ADDREF (Hall et al., 1995)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'Xtal3.4 BONDLA and CIFIO'
_computing_structure_refinement  'Xtal3.4 CRYLSQ'
_computing_structure_solution    Xtal3.4
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .015
_diffrn_reflns_av_sigmaI/netI    .012
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5116
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         29.95
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        .61
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.35
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             452
_exptl_crystal_size_max          .19
_exptl_crystal_size_mid          .11
_exptl_crystal_size_min          .095
_refine_diff_density_max         .539
_refine_diff_density_min         -.529
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.317
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1114
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .029
_refine_ls_R_factor_gt           .017
_refine_ls_shift/esd_max         .001
_refine_ls_shift/esd_mean        .0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
w = WF^.^WS, where WF(Fₒ < 20) = (Fₒ/20)^1.5^,
WF(Fₒ > 22) = (22/Fₒ)¹,
WF(20 < Fₒ<22) = 1,
and WS(sinΘ < 0.48) = (0.48/sinΘ)^2.0^
WS(sinΘ > 0.56) = (sinΘ/0.56)^2.0^
WS(0.48 < sinΘ < 0.56) = 1
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .028
_reflns_number_observed          1114
_reflns_number_total             1358
_reflns_observed_criterion       >3sigma(I)
_cod_data_source_file            na1469.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C14 H18 Cl4 Mo1 N2'
_cod_database_code               2011150
_cod_database_fobs_code          2011150
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,+y,-z
-x,-y,-z
+x,-y,+z
1/2+x,1/2+y,+z
1/2-x,1/2+y,-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,+z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mo .0219(3) .0341(3) .0243(3) .00000 .0059(2) .00000
Cl .0397(5) .0469(6) .0412(6) .0073(4) .0097(4) -.0103(4)
N .0249(18) .039(2) .028(2) .00000 .0040(15) .00000
C1 .028(2) .053(3) .032(3) .00000 .008(2) .00000
C2 .027(2) .053(3) .030(3) .00000 .0059(19) .00000
C3 .027(2) .037(3) .034(3) .00000 .0023(19) .00000
C4 .031(3) .066(4) .031(3) .00000 .005(2) .00000
C5 .033(2) .061(4) .028(3) .00000 .005(2) .00000
C6 .029(2) .066(4) .031(3) .00000 -.003(2) .00000
C7 .041(3) .070(4) .032(3) .00000 -.007(2) .00000
loop_
_atom_site_label
_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_calc_flag
_atom_site_calc_attached_atom
Mo .50000 .50000 .50000 .0265(3) Uani ? ?
Cl .55020(5) .28486(12) .31276(13) .0422(6) Uani ? ?
N .6201(2) .50000 .6875(5) .0306(19) Uani ? ?
C1 .6944(3) .50000 .6173(7) .038(3) Uani ? ?
C2 .7701(3) .50000 .7319(7) .036(2) Uani ? ?
C3 .7738(3) .50000 .9287(7) .033(2) Uani ? ?
C4 .6972(3) .50000 .9985(7) .043(3) Uani ? ?
C5 .6223(3) .50000 .8759(7) .040(3) Uani ? ?
C6 .8580(3) .50000 1.0530(7) .043(3) Uani ? ?
C7 .8538(3) .50000 1.2652(8) .049(3) Uani ? ?
H1 .69150 .50000 .46570 .03600 Uiso ? ?
H2 .82350 .50000 .66820 .03600 Uiso ? ?
H4 .69370 .50000 1.14440 .04300 Uiso ? ?
H5 .56420 .50000 .92540 .04100 Uiso ? ?
H6 .89020 .39770 1.00000 .04400 Uiso ? ?
H71 .82290 .39680 1.30180 .05200 Uiso ? ?
H72 .91190 .50000 1.32900 .05200 Uiso ? ?
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo -1.825 .688 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
Cl .132 .159 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
C .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
N .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
H 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-5 -3 1
-6 -2 2
-4 0 4
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl Mo N . . 90.27(8) yes
Cl Mo Cl . 2_656 90.31(3) yes
Cl Mo N . 2_656 89.73(8) yes
Cl Mo Cl . 3_666 180.0000 no
Cl Mo Cl . 4_565 89.69(3) yes
N Mo Cl . 2_656 89.73(8) no
N Mo N . 2_656 180.0000 no
N Mo Cl . 3_666 89.73(8) no
N Mo Cl . 4_565 90.27(8) no
Cl Mo N 2_656 2_656 90.27(8) no
Cl Mo Cl 2_656 3_666 89.69(3) no
Cl Mo Cl 2_656 4_565 180.0000 no
N Mo Cl 2_656 3_666 90.27(8) no
N Mo Cl 2_656 4_565 89.73(8) no
Cl Mo Cl 3_666 4_565 90.31(3) no
Mo N C1 . . 121.3(3) no
Mo N C5 . . 120.8(3) no
C1 N C5 . . 117.9(4) no
N C1 C2 . . 122.3(5) no
N C1 H1 . . 117.0(4) no
C2 C1 H1 . . 120.7(5) no
C1 C2 C3 . . 120.7(4) no
C1 C2 H2 . . 117.7(5) no
C3 C2 H2 . . 121.7(4) no
C2 C3 C4 . . 116.4(4) no
C2 C3 C6 . . 120.0(4) no
C4 C3 C6 . . 123.6(4) no
C3 C4 C5 . . 120.5(5) no
C3 C4 H4 . . 121.8(4) no
C5 C4 H4 . . 117.7(5) no
N C5 C4 . . 122.2(5) no
N C5 H5 . . 116.1(4) no
C4 C5 H5 . . 121.7(5) no
C3 C6 C7 . . 115.1(4) no
C3 C6 H6 . . 103.7(3) no
C3 C6 H6 . 4_565 103.7(3) no
C7 C6 H6 . . 117.1(3) no
C7 C6 H6 . 4_565 117.1(3) no
H6 C6 H6 . 4_565 97.8(4) no
C6 C7 H71 . . 110.9(3) no
C6 C7 H72 . . 106.9(5) no
C6 C7 H71 . 4_565 110.9(3) no
H71 C7 H72 . . 111.0(3) no
H71 C7 H71 . 4_565 106.2(5) no
H72 C7 H71 . 4_565 111.0(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo Cl . . 2.3396(9) yes
Mo N . . 2.195(3) yes
Mo Cl . 2_656 2.3396(9) no
Mo N . 2_656 2.195(3) no
Mo Cl . 3_666 2.3396(9) no
Mo Cl . 4_565 2.3396(9) no
N C1 . . 1.361(6) no
N C5 . . 1.344(6) no
C1 C2 . . 1.372(6) no
C1 H1 . . 1.079(5) no
C2 C3 . . 1.401(7) no
C2 H2 . . 1.028(5) no
C3 C4 . . 1.394(7) no
C3 C6 . . 1.515(6) no
C4 C5 . . 1.389(6) no
C4 H4 . . 1.054(5) no
C5 H5 . . 1.046(5) no
C6 C7 . . 1.529(8) no
C6 H6 . . 1.041(4) no
C6 H6 . 4_565 1.041(4) no
C7 H71 . . .990(3) no
C7 H72 . . .982(5) no
C7 H71 . 4_565 .990(3) no
