#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179758 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/54/7005464.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_7005464
loop_
_publ_author_name
'Alvarez, Celedonio M.'
'García-Rodríguez, Raúl'
'Miguel, Daniel'
_publ_section_title
;
 Pyridine-2-carboxaldehyde as ligand: synthesis and derivatization of
 carbonyl complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3546
_journal_page_last               3554
_journal_paper_doi               10.1039/b702418e
_journal_year                    2007
_chemical_formula_sum            'C13 H12 F3 Mo N O6 S'
_chemical_formula_weight         463.24
_chemical_name_systematic
;
?
;
_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-97
_cell_angle_alpha                100.666(10)
_cell_angle_beta                 99.137(10)
_cell_angle_gamma                112.880(11)
_cell_formula_units_Z            2
_cell_length_a                   7.834(4)
_cell_length_b                   9.046(5)
_cell_length_c                   14.035(8)
_cell_measurement_temperature    293(2)
_cell_volume                     870.8(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3921
_diffrn_reflns_theta_full        23.35
_diffrn_reflns_theta_max         23.35
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.808560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0374
_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)+(0.0505P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0905
_reflns_number_gt                1956
_reflns_number_total             2491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702418e.txt
_cod_data_source_block           Compound_3d_rg281am
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      P-1
_cod_database_code               7005464
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_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 0.28090(7) 1.09255(5) 0.26786(3) 0.03883(17) Uani 1 1 d . . .
S1 S -0.0283(2) 0.72467(17) 0.28332(10) 0.0480(4) Uani 1 1 d . . .
N1 N 0.3063(6) 0.9107(5) 0.1470(3) 0.0425(10) Uani 1 1 d . . .
C1 C 0.0396(9) 1.0804(6) 0.1986(4) 0.0492(14) Uani 1 1 d . . .
O1 O -0.1011(7) 1.0765(6) 0.1538(3) 0.0765(13) Uani 1 1 d . . .
C2 C 0.3649(9) 1.2577(8) 0.1950(5) 0.0620(17) Uani 1 1 d . . .
O2 O 0.4007(8) 1.3521(6) 0.1474(4) 0.0988(17) Uani 1 1 d . . .
O3 O 0.5531(5) 1.0699(4) 0.3238(2) 0.0486(9) Uani 1 1 d . . .
O11 O 0.1671(5) 0.8573(4) 0.3160(2) 0.0422(8) Uani 1 1 d . . .
O12 O -0.1562(7) 0.7521(6) 0.3382(4) 0.0949(16) Uani 1 1 d . . .
O13 O -0.1035(7) 0.6667(5) 0.1780(3) 0.0831(14) Uani 1 1 d . . .
C3 C 0.1357(9) 1.1819(7) 0.3854(4) 0.0556(16) Uani 1 1 d . . .
H3A H 0.0919 1.2652 0.3738 0.067 Uiso 1 1 calc R . .
H3B H 0.0498 1.0972 0.4107 0.067 Uiso 1 1 calc R . .
C4 C 0.3316(9) 1.2379(6) 0.4255(4) 0.0486(14) Uani 1 1 d . . .
C5 C 0.4515(9) 1.3521(7) 0.3800(4) 0.0637(17) Uani 1 1 d . . .
H5A H 0.5885 1.3888 0.4036 0.076 Uiso 1 1 calc R . .
H5B H 0.4165 1.4397 0.3673 0.076 Uiso 1 1 calc R . .
C6 C 0.4098(10) 1.1740(8) 0.5050(4) 0.0631(17) Uani 1 1 d . . .
H6A H 0.3227 1.0606 0.4975 0.095 Uiso 1 1 calc R . .
H6B H 0.4247 1.2414 0.5700 0.095 Uiso 1 1 calc R . .
H6C H 0.5319 1.1792 0.4984 0.095 Uiso 1 1 calc R . .
C9 C 0.0086(11) 0.5582(8) 0.3204(7) 0.079(2) Uani 1 1 d . . .
C11 C 0.1827(9) 0.8284(7) 0.0575(4) 0.0558(15) Uani 1 1 d . . .
H11 H 0.0857 0.8596 0.0376 0.067 Uiso 1 1 calc R . .
C12 C 0.1933(10) 0.6989(8) -0.0067(4) 0.0703(19) Uani 1 1 d . . .
H12 H 0.1038 0.6438 -0.0684 0.084 Uiso 1 1 calc R . .
C13 C 0.3349(10) 0.6520(8) 0.0204(4) 0.0692(18) Uani 1 1 d . . .
H13 H 0.3433 0.5648 -0.0223 0.083 Uiso 1 1 calc R . .
C14 C 0.4668(9) 0.7364(7) 0.1129(4) 0.0593(16) Uani 1 1 d . . .
H14 H 0.5654 0.7071 0.1330 0.071 Uiso 1 1 calc R . .
C15 C 0.4491(8) 0.8633(6) 0.1738(4) 0.0419(12) Uani 1 1 d . . .
C16 C 0.5773(8) 0.9593(7) 0.2723(4) 0.0466(13) Uani 1 1 d . . .
H16 H 0.6790 0.9360 0.2963 0.056 Uiso 1 1 calc R . .
F1 F -0.1505(6) 0.4181(5) 0.2908(4) 0.1114(16) Uani 1 1 d . . .
F2 F 0.0738(8) 0.5900(6) 0.4159(4) 0.134(2) Uani 1 1 d . . .
F3 F 0.1377(7) 0.5285(5) 0.2770(4) 0.1186(17) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
C2 Mo1 C1 78.3(2) . . ?
C2 Mo1 N1 88.9(2) . . ?
C1 Mo1 N1 97.41(19) . . ?
C2 Mo1 C4 105.2(2) . . ?
C1 Mo1 C4 104.1(2) . . ?
N1 Mo1 C4 156.19(17) . . ?
C2 Mo1 O11 166.01(19) . . ?
C1 Mo1 O11 98.53(18) . . ?
N1 Mo1 O11 77.89(13) . . ?
C4 Mo1 O11 88.80(16) . . ?
C2 Mo1 O3 101.7(2) . . ?
C1 Mo1 O3 169.58(17) . . ?
N1 Mo1 O3 72.20(14) . . ?
C4 Mo1 O3 86.01(17) . . ?
O11 Mo1 O3 78.86(13) . . ?
C2 Mo1 C5 70.8(2) . . ?
C1 Mo1 C5 108.3(2) . . ?
N1 Mo1 C5 142.5(2) . . ?
C4 Mo1 C5 36.6(2) . . ?
O11 Mo1 C5 122.83(17) . . ?
O3 Mo1 C5 81.30(18) . . ?
C2 Mo1 C3 108.5(2) . . ?
C1 Mo1 C3 70.6(2) . . ?
N1 Mo1 C3 155.60(19) . . ?
C4 Mo1 C3 35.34(19) . . ?
O11 Mo1 C3 82.86(16) . . ?
O3 Mo1 C3 118.63(17) . . ?
C5 Mo1 C3 61.5(2) . . ?
O13 S1 O12 114.8(3) . . ?
O13 S1 O11 114.2(2) . . ?
O12 S1 O11 114.7(3) . . ?
O13 S1 C9 105.6(3) . . ?
O12 S1 C9 104.5(3) . . ?
O11 S1 C9 101.0(3) . . ?
C11 N1 C15 117.5(4) . . ?
C11 N1 Mo1 126.5(3) . . ?
C15 N1 Mo1 115.4(3) . . ?
O1 C1 Mo1 176.8(5) . . ?
O2 C2 Mo1 174.8(6) . . ?
C16 O3 Mo1 116.5(3) . . ?
S1 O11 Mo1 127.46(18) . . ?
C4 C3 Mo1 68.4(3) . . ?
C3 C4 C5 114.6(5) . . ?
C3 C4 C6 122.6(5) . . ?
C5 C4 C6 122.6(6) . . ?
C3 C4 Mo1 76.3(3) . . ?
C5 C4 Mo1 74.1(3) . . ?
C6 C4 Mo1 114.7(3) . . ?
C4 C5 Mo1 69.3(3) . . ?
F2 C9 F1 108.1(6) . . ?
F2 C9 F3 106.9(6) . . ?
F1 C9 F3 106.9(6) . . ?
F2 C9 S1 113.5(5) . . ?
F1 C9 S1 111.7(5) . . ?
F3 C9 S1 109.5(5) . . ?
N1 C11 C12 122.5(5) . . ?
C13 C12 C11 119.8(6) . . ?
C12 C13 C14 119.0(5) . . ?
C15 C14 C13 118.8(5) . . ?
C14 C15 N1 122.4(5) . . ?
C14 C15 C16 123.7(5) . . ?
N1 C15 C16 113.9(4) . . ?
O3 C16 C15 120.8(5) . . ?
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 C2 1.930(6) . ?
Mo1 C1 1.935(6) . ?
Mo1 N1 2.226(4) . ?
Mo1 C4 2.241(5) . ?
Mo1 O11 2.242(3) . ?
Mo1 O3 2.253(4) . ?
Mo1 C5 2.302(6) . ?
Mo1 C3 2.342(5) . ?
S1 O13 1.415(4) . ?
S1 O12 1.424(4) . ?
S1 O11 1.462(4) . ?
S1 C9 1.789(6) . ?
N1 C11 1.332(6) . ?
N1 C15 1.370(6) . ?
C1 O1 1.163(6) . ?
C2 O2 1.156(6) . ?
O3 C16 1.218(5) . ?
C3 C4 1.394(8) . ?
C4 C5 1.427(8) . ?
C4 C6 1.501(7) . ?
C9 F2 1.292(8) . ?
C9 F1 1.321(8) . ?
C9 F3 1.346(8) . ?
C11 C12 1.378(7) . ?
C12 C13 1.359(8) . ?
C13 C14 1.389(8) . ?
C14 C15 1.365(7) . ?
C15 C16 1.453(7) . ?
