#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:26:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179896 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/92/7019219.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_7019219
loop_
_publ_author_name
'Arroyo, Marta'
'Miguel, Daniel'
'Villafañe, Fernando'
'Alegria, Elisabete C. B.'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Molybdenum- and tungsten(ii) monometallic 3-(2-pyridyl)pyrazole and
 bimetallic 3-(2-pyridyl)pyrazolate complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7017
_journal_page_last               7025
_journal_paper_doi               10.1039/c2dt12388f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C26 H22 Mo2 N6 O4'
_chemical_formula_weight         674.38
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   18.316(10)
_cell_length_b                   18.316(9)
_cell_length_c                   42.269(10)
_cell_measurement_reflns_used    743
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.39
_cell_measurement_theta_min      2.22
_cell_volume                     12280(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.1274
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            17301
_diffrn_reflns_theta_full        23.44
_diffrn_reflns_theta_max         23.44
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.718393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             6048
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.782
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         1967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0573
_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)+(0.1013P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                1295
_reflns_number_total             1967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12388f.txt
_cod_data_source_block           Compound_6_ma1691am
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        12280(14)
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7019219
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Mo1 Mo 0.79156(6) 0.76857(6) 0.07399(2) 0.0332(4) Uani 1 1 d .
N2 N 0.6843(5) 0.6515(5) 0.0510(2) 0.033(2) Uani 1 1 d .
N1 N 0.8422(6) 0.6844(6) 0.0549(2) 0.042(2) Uani 1 1 d .
N3 N 0.5997(5) 0.6117(5) 0.0533(2) 0.033(2) Uani 1 1 d .
C1 C 0.8866(8) 0.8421(8) 0.1003(4) 0.062(4) Uani 1 1 d .
O1 O 0.9402(7) 0.8818(6) 0.1188(4) 0.107(5) Uani 1 1 d .
C2 C 0.7560(7) 0.8406(7) 0.0937(3) 0.038(3) Uani 1 1 d .
O2 O 0.7440(5) 0.8915(5) 0.1062(2) 0.057(2) Uani 1 1 d .
C3 C 0.9023(9) 0.8639(9) 0.0419(4) 0.068(4) Uani 1 1 d .
H3A H 0.9247 0.9233 0.0463 0.04(3) Uiso 1 1 calc R
H3B H 0.9451 0.8496 0.0366 0.06(4) Uiso 1 1 calc R
C4 C 0.8274(9) 0.8233(9) 0.0249(3) 0.058(4) Uani 1 1 d .
H4 H 0.8207 0.7883 0.0063 0.15(8) Uiso 1 1 calc R
C5 C 0.7652(8) 0.8402(8) 0.0345(3) 0.049(3) Uani 1 1 d .
H5A H 0.7112 0.8095 0.0238 0.12(6) Uiso 1 1 calc R
H5B H 0.7826 0.8987 0.0387 0.03(3) Uiso 1 1 calc R
C11 C 0.9220(8) 0.7010(9) 0.0578(3) 0.054(4) Uani 1 1 d .
H11 H 0.9576 0.7442 0.0714 0.02(3) Uiso 1 1 calc R
C12 C 0.9534(10) 0.6592(10) 0.0423(4) 0.066(4) Uani 1 1 d .
H12 H 1.0089 0.6725 0.0454 0.05(4) Uiso 1 1 calc R
C13 C 0.9043(11) 0.5989(11) 0.0225(3) 0.071(5) Uani 1 1 d .
H13 H 0.9255 0.5706 0.0108 0.06(4) Uiso 1 1 calc R
C14 C 0.8231(10) 0.5785(9) 0.0194(3) 0.057(4) Uani 1 1 d .
H14 H 0.7876 0.5348 0.0060 0.03(3) Uiso 1 1 calc R
C15 C 0.7926(8) 0.6218(8) 0.0360(3) 0.043(3) Uani 1 1 d .
C16 C 0.7051(8) 0.6015(7) 0.0351(3) 0.038(3) Uani 1 1 d .
C17 C 0.6311(8) 0.5290(7) 0.0256(3) 0.051(3) Uani 1 1 d .
H17 H 0.6264 0.4842 0.0137 0.03(3) Uiso 1 1 calc R
C18 C 0.5693(8) 0.5382(8) 0.0375(3) 0.047(3) Uani 1 1 d .
H18 H 0.5123 0.4991 0.0352 0.04(3) Uiso 1 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'
O O 0.0106 0.0060 '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
C2 Mo1 C1 76.6(5) . .
C2 Mo1 N3 89.1(4) . 18_654
C1 Mo1 N3 90.9(5) . 18_654
C2 Mo1 C4 102.5(5) . .
C1 Mo1 C4 105.0(6) . .
N3 Mo1 C4 162.0(5) 18_654 .
C2 Mo1 N2 113.6(4) . .
C1 Mo1 N2 162.5(5) . .
N3 Mo1 N2 75.7(3) 18_654 .
C4 Mo1 N2 87.0(5) . .
C2 Mo1 N1 174.2(4) . .
C1 Mo1 N1 98.3(5) . .
N3 Mo1 N1 88.2(3) 18_654 .
C4 Mo1 N1 81.4(4) . .
N2 Mo1 N1 70.6(3) . .
C2 Mo1 C5 71.8(5) . .
C1 Mo1 C5 113.0(6) . .
N3 Mo1 C5 143.9(4) 18_654 .
C4 Mo1 C5 35.2(4) . .
N2 Mo1 C5 84.2(4) . .
N1 Mo1 C5 113.2(4) . .
C2 Mo1 C3 101.7(5) . .
C1 Mo1 C3 70.8(6) . .
N3 Mo1 C3 155.5(5) 18_654 .
C4 Mo1 C3 35.2(5) . .
N2 Mo1 C3 118.3(5) . .
N1 Mo1 C3 78.9(4) . .
C5 Mo1 C3 60.5(5) . .
C16 N2 N3 108.1(9) . .
C16 N2 Mo1 116.8(7) . .
N3 N2 Mo1 134.2(7) . .
C15 N1 C11 116.9(11) . .
C15 N1 Mo1 117.4(8) . .
C11 N1 Mo1 125.0(9) . .
N2 N3 C18 107.1(9) . .
N2 N3 Mo1 119.2(6) . 18_654
C18 N3 Mo1 128.8(8) . 18_654
O1 C1 Mo1 173.5(15) . .
O2 C2 Mo1 172.2(10) . .
C4 C3 Mo1 69.2(7) . .
C5 C4 C3 115.5(14) . .
C5 C4 Mo1 74.9(7) . .
C3 C4 Mo1 75.6(8) . .
C4 C5 Mo1 69.9(7) . .
C12 C11 N1 123.9(15) . .
C13 C12 C11 118.9(15) . .
C12 C13 C14 119.3(13) . .
C13 C14 C15 120.3(15) . .
N1 C15 C14 120.6(12) . .
N1 C15 C16 115.5(10) . .
C14 C15 C16 123.8(12) . .
N2 C16 C17 108.8(10) . .
N2 C16 C15 118.0(10) . .
C17 C16 C15 132.1(11) . .
C18 C17 C16 104.7(11) . .
C17 C18 N3 111.3(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 C2 1.928(12) .
Mo1 C1 1.933(14) .
Mo1 N3 2.205(9) 18_654
Mo1 C4 2.255(13) .
Mo1 N2 2.278(9) .
Mo1 N1 2.306(9) .
Mo1 C5 2.317(12) .
Mo1 C3 2.337(13) .
N2 C16 1.335(14) .
N2 N3 1.345(11) .
N1 C15 1.318(15) .
N1 C11 1.341(15) .
N3 C18 1.349(14) .
N3 Mo1 2.205(9) 18_654
C1 O1 1.179(16) .
C2 O2 1.183(13) .
C3 C4 1.39(2) .
C4 C5 1.383(18) .
C11 C12 1.335(18) .
C12 C13 1.32(2) .
C13 C14 1.35(2) .
C14 C15 1.370(17) .
C15 C16 1.453(16) .
C16 C17 1.402(17) .
C17 C18 1.323(17) .
