#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/21/7012115.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_7012115
loop_
_publ_author_name
'Barbara Modec'
'Jurij V. Brenčič'
'Darko Dolenc'
'Jon Zubieta'
_publ_section_title
;
 The first oxalate-bridged one-dimensional polymer containing Mo dimers
 with single metal--metal bonds. Syntheses and structures of
 (MeNC5H5)2n[Mo2O4(C2O4)Cl2]n and (3-MePyH)2n[Mo2O4(C2O4)Cl2]n
;
_journal_issue                   24
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4582
_journal_page_last               4586
_journal_paper_doi               10.1039/b207544j
_journal_year                    2002
_chemical_formula_sum            'C14 H16 Cl2 Mo2 N2 O8'
_chemical_formula_weight         603.07
_chemical_name_systematic
; 
N-methylpyridinium dichlorooxalatotetraoxodimolybdate(V) 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 120.073(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.068(3)
_cell_length_b                   8.8105(12)
_cell_length_c                   12.466(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1907.4(5)
_computing_cell_refinement       'SMART (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SMART (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART diffractometer'
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6166
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    1.641
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0478P)²+0.2337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0808
_reflns_number_gt                1926
_reflns_number_total             2296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207544j.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7012115
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
Mo Mo 0.468083(15) 0.76279(3) 0.13167(2) 0.00905(10) Uani 1 1 d . . .
Cl Cl 0.33894(4) 0.81674(9) -0.04551(7) 0.01416(17) Uani 1 1 d . . .
O1 O 0.46336(12) 0.5756(2) 0.10314(19) 0.0137(5) Uani 1 1 d . . .
O2 O 0.42670(13) 0.8014(3) 0.23833(19) 0.0120(4) Uani 1 1 d . . .
O3 O 0.47259(12) 1.0227(2) 0.11077(18) 0.0115(5) Uani 1 1 d . . .
O4 O 0.50893(13) 0.8036(2) 0.0025(2) 0.0121(5) Uani 1 1 d . . .
C4 C 0.51039(16) 0.9373(3) -0.0316(3) 0.0093(6) Uani 1 1 d . . .
N1 N 0.17266(17) 0.2314(3) -0.1821(2) 0.0163(6) Uani 1 1 d . . .
C11 C 0.1612(2) 0.3828(4) -0.1781(3) 0.0174(7) Uani 1 1 d . . .
H11 H 0.116(2) 0.395(4) -0.192(3) 0.024(11) Uiso 1 1 d . . .
C12 C 0.2215(2) 0.4808(4) -0.1377(3) 0.0182(7) Uani 1 1 d . . .
H12 H 0.209(2) 0.581(5) -0.133(3) 0.032(12) Uiso 1 1 d . . .
C13 C 0.2932(2) 0.4267(4) -0.1041(3) 0.0224(8) Uani 1 1 d . . .
H13 H 0.332(2) 0.486(5) -0.080(4) 0.032(12) Uiso 1 1 d . . .
C14 C 0.3044(2) 0.2744(5) -0.1097(3) 0.0240(8) Uani 1 1 d . . .
H14 H 0.348(3) 0.236(5) -0.084(5) 0.044(15) Uiso 1 1 d . . .
C15 C 0.2433(2) 0.1780(4) -0.1486(3) 0.0192(8) Uani 1 1 d . . .
H15 H 0.248(2) 0.099(5) -0.150(3) 0.018(11) Uiso 1 1 d . . .
C16 C 0.1062(3) 0.1272(5) -0.2290(4) 0.0305(9) Uani 1 1 d . . .
H16C H 0.075(3) 0.130(5) -0.328(4) 0.052(14) Uiso 1 1 d . . .
H16B H 0.130(3) 0.027(7) -0.179(5) 0.085(19) Uiso 1 1 d . . .
H16A H 0.075(3) 0.164(6) -0.188(4) 0.056(15) Uiso 1 1 d . . .
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 Mo O2 108.84(10) . . ?
O1 Mo O2 105.74(10) . 2_655 ?
O2 Mo O2 93.31(10) . 2_655 ?
O1 Mo O4 90.45(9) . . ?
O2 Mo O4 160.01(9) . . ?
O2 Mo O4 86.16(9) 2_655 . ?
O1 Mo O3 161.80(9) . . ?
O2 Mo O3 87.55(8) . . ?
O2 Mo O3 80.37(8) 2_655 . ?
O4 Mo O3 72.65(7) . . ?
O1 Mo Cl 94.42(8) . . ?
O2 Mo Cl 87.76(7) . . ?
O2 Mo Cl 158.22(7) 2_655 . ?
O4 Mo Cl 85.51(6) . . ?
O3 Mo Cl 77.94(6) . . ?
O1 Mo Mo 100.75(7) . 2_655 ?
O2 Mo Mo 48.84(7) . 2_655 ?
O2 Mo Mo 48.05(6) 2_655 2_655 ?
O4 Mo Mo 134.22(6) . 2_655 ?
O3 Mo Mo 96.00(5) . 2_655 ?
Cl Mo Mo 136.57(3) . 2_655 ?
Mo O2 Mo 83.10(9) . 2_655 ?
C4 O3 Mo 114.28(18) 5_675 . ?
C4 O4 Mo 119.18(19) . . ?
O3 C4 O4 126.5(3) 5_675 . ?
O3 C4 C4 117.2(3) 5_675 5_675 ?
O4 C4 C4 116.3(3) . 5_675 ?
C15 N1 C11 120.2(3) . . ?
C15 N1 C16 120.5(3) . . ?
C11 N1 C16 119.3(3) . . ?
N1 C11 C12 120.1(3) . . ?
C11 C12 C13 119.8(3) . . ?
C12 C13 C14 120.0(4) . . ?
C15 C14 C13 119.2(4) . . ?
N1 C15 C14 120.7(3) . . ?
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
Mo O1 1.680(2) . ?
Mo O2 1.918(2) . ?
Mo O2 1.942(2) 2_655 ?
Mo O4 2.171(2) . ?
Mo O3 2.312(2) . ?
Mo Cl 2.4666(8) . ?
Mo Mo 2.5607(7) 2_655 ?
O2 Mo 1.942(2) 2_655 ?
O3 C4 1.246(3) 5_675 ?
O4 C4 1.257(4) . ?
C4 O3 1.246(3) 5_675 ?
C4 C4 1.532(6) 5_675 ?
N1 C15 1.346(5) . ?
N1 C11 1.359(4) . ?
N1 C16 1.477(5) . ?
C11 C12 1.361(5) . ?
C12 C13 1.368(5) . ?
C13 C14 1.368(6) . ?
C14 C15 1.366(6) . ?
