#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:18:41 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180499 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/68/7216865.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_7216865
loop_
_publ_author_name
'Liang, Ji-Lei'
'Lu, Yu-Kun'
'Zhao, Jin-chong'
'Li, Xue-Hui'
'Pan, Yuan'
'Wu, Meng-Meng'
'Liu, Yun-Qi'
'Liu, Chen-Guang'
_publ_section_title
;
 A novel POMos-based hybrid with penta-coordinated Mo in trigonal
 bipyramid: structure and an efficient precursor for hydrodesulfurization
 catalyst
;
_journal_issue                   53
_journal_name_full               'RSC Advances'
_journal_page_first              27787
_journal_paper_doi               10.1039/c4ra02696a
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C15 H12 Mo2 N3 Ni O7'
_chemical_formula_sum            'C15 H12 Mo2 N3 Ni O7'
_chemical_formula_weight         596.87
_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                98.021(8)
_cell_angle_beta                 90.098(6)
_cell_angle_gamma                106.227(8)
_cell_formula_units_Z            2
_cell_length_a                   7.1747(5)
_cell_length_b                   11.1258(13)
_cell_length_c                   11.4017(8)
_cell_measurement_temperature    293(2)
_cell_volume                     864.53(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4971
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0370
_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)+(0.0386P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                2291
_reflns_number_total             3110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra02696a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        864.53(13)
_cod_database_code               7216865
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
Mo1 Mo 1.24845(5) 0.09589(4) 0.27205(3) 0.01241(14) Uani 1 1 d .
Mo2 Mo 0.75984(5) -0.09719(4) 0.22727(3) 0.01273(14) Uani 1 1 d .
Ni1 Ni 0.5000 0.0000 0.5000 0.0124(2) Uani 1 2 d S
Ni2 Ni 0.5000 0.0000 0.0000 0.0122(2) Uani 1 2 d S
O2 O 1.3716(4) 0.0508(3) 0.1485(3) 0.0207(8) Uani 1 1 d .
O3 O 1.3313(4) 0.0913(3) 0.4165(3) 0.0185(8) Uani 1 1 d .
O4 O 1.0259(4) -0.0549(3) 0.2573(3) 0.0220(8) Uani 1 1 d .
O7 O 0.6449(4) -0.0358(3) 0.3466(3) 0.0202(8) Uani 1 1 d .
O6 O 0.7088(5) -0.0426(3) 0.0988(3) 0.0218(8) Uani 1 1 d .
O1 O 1.1174(4) 0.2027(4) 0.2592(3) 0.0269(9) Uani 1 1 d .
O5 O 0.6712(5) -0.2596(3) 0.2059(3) 0.0262(9) Uani 1 1 d .
N1 N 1.5059(6) 0.2783(4) 0.2943(4) 0.0193(10) Uani 1 1 d .
N2 N 2.2789(5) 0.8352(4) 0.4505(3) 0.0169(9) Uani 1 1 d .
N3 N 0.3152(6) -0.1884(4) -0.0049(3) 0.0194(10) Uani 1 1 d .
C1 C 1.6900(7) 0.2742(5) 0.2941(4) 0.0216(12) Uani 1 1 d .
H1 H 1.7153 0.1963 0.2762 0.026 Uiso 1 1 calc R
C2 C 1.8434(7) 0.3816(5) 0.3195(4) 0.0236(12) Uani 1 1 d .
H2 H 1.9696 0.3748 0.3195 0.028 Uiso 1 1 calc R
C3 C 1.8131(7) 0.4989(5) 0.3449(4) 0.0209(12) Uani 1 1 d .
C4 C 1.6204(7) 0.5020(5) 0.3410(6) 0.0365(16) Uani 1 1 d .
H4 H 1.5904 0.5787 0.3550 0.044 Uiso 1 1 calc R
C5 C 1.4759(7) 0.3908(6) 0.3162(5) 0.0364(16) Uani 1 1 d .
H5 H 1.3481 0.3947 0.3147 0.044 Uiso 1 1 calc R
C6 C 2.3103(7) 0.7340(5) 0.3854(5) 0.0273(13) Uani 1 1 d .
H6 H 2.4365 0.7369 0.3646 0.033 Uiso 1 1 calc R
C7 C 2.1626(7) 0.6248(5) 0.3475(5) 0.0266(13) Uani 1 1 d .
H7 H 2.1906 0.5566 0.3015 0.032 Uiso 1 1 calc R
C8 C 1.9726(7) 0.6170(5) 0.3781(4) 0.0199(12) Uani 1 1 d .
C9 C 1.9419(7) 0.7229(5) 0.4445(4) 0.0203(12) Uani 1 1 d .
H9 H 1.8173 0.7223 0.4675 0.024 Uiso 1 1 calc R
C10 C 2.0950(7) 0.8294(5) 0.4768(4) 0.0185(12) Uani 1 1 d .
H10 H 2.0695 0.9005 0.5189 0.022 Uiso 1 1 calc R
C11 C 0.3818(7) -0.2884(5) -0.0124(5) 0.0265(13) Uani 1 1 d .
H11 H 0.5151 -0.2755 -0.0178 0.032 Uiso 1 1 calc R
C12 C 0.2668(7) -0.4105(5) -0.0127(5) 0.0300(14) Uani 1 1 d .
H12 H 0.3226 -0.4771 -0.0204 0.036 Uiso 1 1 calc R
C13 C 0.0655(7) -0.4344(5) -0.0014(4) 0.0212(12) Uani 1 1 d .
C14 C -0.0026(8) -0.3295(6) 0.0064(5) 0.0348(15) Uani 1 1 d .
H14 H -0.1349 -0.3391 0.0136 0.042 Uiso 1 1 calc R
C15 C 0.1220(7) -0.2103(6) 0.0039(5) 0.0296(14) Uani 1 1 d .
H15 H 0.0700 -0.1421 0.0084 0.036 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'
Mo Mo -1.6832 0.6857 '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'
Ni Ni 0.3393 1.1124 '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
O1 Mo1 O2 118.03(17) . .
O1 Mo1 O3 116.16(17) . .
O2 Mo1 O3 120.53(15) . .
O1 Mo1 O4 96.55(15) . .
O2 Mo1 O4 98.18(15) . .
O3 Mo1 O4 98.28(14) . .
O1 Mo1 N1 81.99(15) . .
O2 Mo1 N1 83.85(15) . .
O3 Mo1 N1 81.08(14) . .
O4 Mo1 N1 177.90(15) . .
O5 Mo2 O6 108.19(16) . .
O5 Mo2 O7 108.80(17) . .
O6 Mo2 O7 110.08(16) . .
O5 Mo2 O4 108.21(16) . .
O6 Mo2 O4 110.34(15) . .
O7 Mo2 O4 111.14(14) . .
N2 Ni1 N2 180.0 2_866 1_345
N2 Ni1 O7 90.79(14) 2_866 2_656
N2 Ni1 O7 89.21(14) 1_345 2_656
N2 Ni1 O7 89.21(14) 2_866 .
N2 Ni1 O7 90.79(14) 1_345 .
O7 Ni1 O7 180.0 2_656 .
N2 Ni1 O3 93.42(14) 2_866 1_455
N2 Ni1 O3 86.58(14) 1_345 1_455
O7 Ni1 O3 86.92(13) 2_656 1_455
O7 Ni1 O3 93.08(13) . 1_455
N2 Ni1 O3 86.58(14) 2_866 2_756
N2 Ni1 O3 93.42(14) 1_345 2_756
O7 Ni1 O3 93.08(13) 2_656 2_756
O7 Ni1 O3 86.92(13) . 2_756
O3 Ni1 O3 180.00(15) 1_455 2_756
O2 Ni2 O2 180.000(1) 1_455 2_755
O2 Ni2 O6 88.92(13) 1_455 2_655
O2 Ni2 O6 91.08(13) 2_755 2_655
O2 Ni2 O6 91.08(13) 1_455 .
O2 Ni2 O6 88.92(13) 2_755 .
O6 Ni2 O6 180.0(2) 2_655 .
O2 Ni2 N3 91.54(14) 1_455 2_655
O2 Ni2 N3 88.46(14) 2_755 2_655
O6 Ni2 N3 90.34(14) 2_655 2_655
O6 Ni2 N3 89.66(14) . 2_655
O2 Ni2 N3 88.46(14) 1_455 .
O2 Ni2 N3 91.54(14) 2_755 .
O6 Ni2 N3 89.66(14) 2_655 .
O6 Ni2 N3 90.34(14) . .
N3 Ni2 N3 180.0(2) 2_655 .
Mo1 O2 Ni2 176.48(19) . 1_655
Mo1 O3 Ni1 138.7(2) . 1_655
Mo2 O4 Mo1 138.2(2) . .
Mo2 O7 Ni1 167.9(2) . .
Mo2 O6 Ni2 145.9(2) . .
C5 N1 C1 117.2(4) . .
C5 N1 Mo1 120.9(3) . .
C1 N1 Mo1 121.7(4) . .
C6 N2 C10 117.3(4) . .
C6 N2 Ni1 122.0(3) . 1_765
C10 N2 Ni1 120.6(4) . 1_765
C11 N3 C15 116.3(5) . .
C11 N3 Ni2 123.0(3) . .
C15 N3 Ni2 120.7(4) . .
N1 C1 C2 122.0(5) . .
N1 C1 H1 119.0 . .
C2 C1 H1 119.0 . .
C3 C2 C1 121.0(5) . .
C3 C2 H2 119.5 . .
C1 C2 H2 119.5 . .
C2 C3 C4 116.2(5) . .
C2 C3 C8 123.2(5) . .
C4 C3 C8 120.6(5) . .
C5 C4 C3 119.2(5) . .
C5 C4 H4 120.4 . .
C3 C4 H4 120.4 . .
N1 C5 C4 124.3(5) . .
N1 C5 H5 117.9 . .
C4 C5 H5 117.9 . .
N2 C6 C7 122.8(5) . .
N2 C6 H6 118.6 . .
C7 C6 H6 118.6 . .
C6 C7 C8 120.0(5) . .
C6 C7 H7 120.0 . .
C8 C7 H7 120.0 . .
C9 C8 C7 116.6(5) . .
C9 C8 C3 121.9(5) . .
C7 C8 C3 121.4(5) . .
C10 C9 C8 120.2(5) . .
C10 C9 H9 119.9 . .
C8 C9 H9 119.9 . .
N2 C10 C9 123.0(5) . .
N2 C10 H10 118.5 . .
C9 C10 H10 118.5 . .
N3 C11 C12 124.3(5) . .
N3 C11 H11 117.9 . .
C12 C11 H11 117.9 . .
C11 C12 C13 120.0(5) . .
C11 C12 H12 120.0 . .
C13 C12 H12 120.0 . .
C14 C13 C12 115.2(5) . .
C14 C13 C13 122.8(6) . 2_545
C12 C13 C13 122.0(6) . 2_545
C13 C14 C15 121.2(5) . .
C13 C14 H14 119.4 . .
C15 C14 H14 119.4 . .
N3 C15 C14 123.0(6) . .
N3 C15 H15 118.5 . .
C14 C15 H15 118.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.730(3) .
Mo1 O2 1.753(3) .
Mo1 O3 1.762(3) .
Mo1 O4 1.953(3) .
Mo1 N1 2.314(4) .
Mo2 O5 1.722(4) .
Mo2 O6 1.738(3) .
Mo2 O7 1.748(3) .
Mo2 O4 1.853(3) .
Ni1 N2 2.068(4) 2_866
Ni1 N2 2.068(4) 1_345
Ni1 O7 2.084(3) 2_656
Ni1 O7 2.084(3) .
Ni1 O3 2.087(3) 1_455
Ni1 O3 2.087(3) 2_756
Ni2 O2 2.016(3) 1_455
Ni2 O2 2.016(3) 2_755
Ni2 O6 2.068(3) 2_655
Ni2 O6 2.068(3) .
Ni2 N3 2.138(4) 2_655
Ni2 N3 2.138(4) .
O2 Ni2 2.016(3) 1_655
O3 Ni1 2.087(3) 1_655
N1 C5 1.318(7) .
N1 C1 1.334(6) .
N2 C6 1.334(7) .
N2 C10 1.340(6) .
N2 Ni1 2.068(4) 1_765
N3 C11 1.321(7) .
N3 C15 1.345(6) .
C1 C2 1.375(7) .
C1 H1 0.9300 .
C2 C3 1.374(7) .
C2 H2 0.9300 .
C3 C4 1.393(7) .
C3 C8 1.483(7) .
C4 C5 1.368(7) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C7 1.385(7) .
C6 H6 0.9300 .
C7 C8 1.389(7) .
C7 H7 0.9300 .
C8 C9 1.382(7) .
C9 C10 1.377(7) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.379(7) .
C11 H11 0.9300 .
C12 C13 1.403(7) .
C12 H12 0.9300 .
C13 C14 1.378(8) .
C13 C13 1.504(9) 2_545
C14 C15 1.380(7) .
C14 H14 0.9300 .
C15 H15 0.9300 .
