#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:29:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180508 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/77/7217762.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_7217762
loop_
_publ_author_name
'Pisk, Jana'
'Prugovečki, Biserka'
'Matković-Čalogović, Dubravka'
'Jednačak, Tomislav'
'Novak, Predrag'
'Agustin, Dominique'
'Vrdoljak, Visnja'
_publ_section_title
;
 Pyridoxal hydrazonato molybdenum(VI) complexes: Assembly, Structure and
 Epoxidation (Pre)Catalyst testing under solvent-free conditions
;
_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/C4RA08179J
_journal_year                    2014
_chemical_formula_sum            'C17 H21 Mo N3 O8'
_chemical_formula_weight         491.31
_chemical_name_systematic
;
cis-(N-((3-oxy)-5-(hydroxymethyl)-2
-methylpyridin-4-yl)methylene)-4-
hydroxylbenzhydrazonato-methanol-
dioxo-molybdenum(VI) methanol solvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                92.297(8)
_cell_angle_beta                 103.058(5)
_cell_angle_gamma                95.262(5)
_cell_formula_units_Z            2
_cell_length_a                   7.8373(5)
_cell_length_b                   9.3588(4)
_cell_length_c                   13.025(3)
_cell_measurement_temperature    150(2)
_cell_volume                     924.9(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2010)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction,2010)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2010)'
_computing_molecular_graphics    'PLATON98 (Spek, 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11816
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         4.272
_exptl_absorpt_coefficient_mu    0.763
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       needle
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         3971
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0301P)²+0.1520P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3673
_reflns_number_total             3971
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ra08179j2.cif
_cod_data_source_block           shelx
_cod_database_code               7217762
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
C1 C 0.7351(2) 0.01451(17) 0.13608(13) 0.0124(3) Uani 1 1 d .
C2 C 0.7408(2) 0.00817(17) -0.12298(13) 0.0129(3) Uani 1 1 d .
C3 C 0.7760(2) 0.10163(17) -0.20384(13) 0.0128(3) Uani 1 1 d .
C4 C 0.8015(2) 0.04074(18) -0.29994(13) 0.0146(3) Uani 1 1 d .
C5 C 0.8206(2) 0.13198(18) -0.37748(14) 0.0162(3) Uani 1 1 d .
C6 C 0.7843(2) 0.33440(17) -0.28056(13) 0.0135(3) Uani 1 1 d .
C7 C 0.7761(2) 0.25144(17) -0.19296(13) 0.0128(3) Uani 1 1 d .
C8 C 0.7609(2) 0.49105(18) -0.27492(14) 0.0163(3) Uani 1 1 d .
C9 C 0.8017(2) -0.11906(18) -0.32048(14) 0.0166(3) Uani 1 1 d .
C10 C 0.7156(2) -0.07796(17) 0.22191(13) 0.0132(3) Uani 1 1 d .
C11 C 0.6687(2) -0.02313(18) 0.31191(13) 0.0149(3) Uani 1 1 d .
C12 C 0.6413(2) -0.11214(19) 0.39003(13) 0.0163(3) Uani 1 1 d .
C13 C 0.6644(2) -0.25741(18) 0.38077(13) 0.0157(3) Uani 1 1 d .
C14 C 0.7125(2) -0.31349(18) 0.29165(14) 0.0170(3) Uani 1 1 d .
C15 C 0.7371(2) -0.22462(18) 0.21312(13) 0.0147(3) Uani 1 1 d .
C16 C 0.4565(3) 0.3668(2) 0.09647(16) 0.0197(4) Uani 1 1 d .
C17 C 0.8728(3) 0.3689(2) 0.39768(18) 0.0290(4) Uani 1 1 d .
N1 N 0.70243(18) -0.04513(14) 0.04009(11) 0.0126(3) Uani 1 1 d .
N2 N 0.73716(17) 0.05643(14) -0.02968(10) 0.0113(3) Uani 1 1 d .
N3 N 0.80724(19) 0.27461(15) -0.36999(11) 0.0151(3) Uani 1 1 d .
O1 O 0.78169(15) 0.15217(12) 0.15825(9) 0.0148(2) Uani 1 1 d .
O2 O 0.75815(15) 0.32152(11) -0.10499(9) 0.0139(2) Uani 1 1 d .
O3 O 0.62628(18) -0.18598(13) -0.33633(11) 0.0239(3) Uani 1 1 d D
O4 O 1.03581(16) 0.25115(13) 0.05262(10) 0.0192(3) Uani 1 1 d .
O5 O 0.83215(15) 0.44276(12) 0.11094(9) 0.0166(2) Uani 1 1 d .
O6 O 0.52838(16) 0.28403(13) 0.02398(9) 0.0147(2) Uani 1 1 d .
O7 O 0.63822(18) -0.33988(15) 0.46051(10) 0.0204(3) Uani 1 1 d .
O8 O 0.72498(18) 0.39539(14) 0.44003(10) 0.0217(3) Uani 1 1 d D
Mo Mo 0.82270(2) 0.28236(2) 0.04255(2) 0.01130(5) Uani 1 1 d .
H2 H 0.717(2) -0.089(2) -0.1375(15) 0.015(5) Uiso 1 1 d .
H3 H 0.610(3) -0.2455(19) -0.3870(13) 0.032(6) Uiso 1 1 d D
H5 H 0.840(3) 0.095(2) -0.4422(16) 0.015(5) Uiso 1 1 d .
H6 H 0.466(3) 0.215(2) 0.0059(18) 0.026(6) Uiso 1 1 d .
H7 H 0.660(3) -0.413(3) 0.454(2) 0.041(8) Uiso 1 1 d .
H8 H 0.747(3) 0.370(2) 0.5011(10) 0.030(6) Uiso 1 1 d D
H8A H 0.839(3) 0.537(2) -0.2139(17) 0.020(5) Uiso 1 1 d .
H8B H 0.653(3) 0.507(2) -0.2687(16) 0.020(5) Uiso 1 1 d .
H8C H 0.781(3) 0.531(2) -0.3371(19) 0.035(6) Uiso 1 1 d .
H9A H 0.880(3) -0.161(2) -0.2662(16) 0.015(5) Uiso 1 1 d .
H9B H 0.844(3) -0.132(2) -0.3820(17) 0.018(5) Uiso 1 1 d .
H11 H 0.648(3) 0.064(2) 0.3169(16) 0.017(5) Uiso 1 1 d .
H12 H 0.600(3) -0.084(2) 0.4447(18) 0.026(6) Uiso 1 1 d .
H14 H 0.729(2) -0.409(2) 0.2847(15) 0.014(5) Uiso 1 1 d .
H15 H 0.769(3) -0.260(2) 0.1554(16) 0.016(5) Uiso 1 1 d .
H16A H 0.483(3) 0.330(2) 0.1676(19) 0.030(6) Uiso 1 1 d .
H16B H 0.506(3) 0.460(3) 0.0978(18) 0.030(6) Uiso 1 1 d .
H16C H 0.337(3) 0.359(2) 0.0720(17) 0.029(6) Uiso 1 1 d .
H17A H 0.950(4) 0.460(3) 0.401(2) 0.052(8) Uiso 1 1 d .
H17B H 0.941(5) 0.294(4) 0.431(3) 0.083(11) Uiso 1 1 d .
H17C H 0.839(4) 0.337(3) 0.333(2) 0.054(8) 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'
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
O1 C1 N1 123.03(15)
O1 C1 C10 119.00(14)
N1 C1 C10 117.97(14)
N2 C2 C3 122.62(15)
C7 C3 C4 118.02(15)
C7 C3 C2 122.22(14)
C4 C3 C2 119.66(14)
C5 C4 C3 117.79(15)
C5 C4 C9 119.75(15)
C3 C4 C9 122.42(15)
N3 C5 C4 124.10(15)
N3 C6 C7 121.09(14)
N3 C6 C8 118.71(15)
C7 C6 C8 120.16(15)
O2 C7 C3 123.46(14)
O2 C7 C6 116.98(14)
C3 C7 C6 119.44(15)
O3 C9 C4 108.98(13)
C11 C10 C15 118.74(15)
C11 C10 C1 120.86(14)
C15 C10 C1 120.36(15)
C12 C11 C10 120.69(15)
C11 C12 C13 120.01(16)
O7 C13 C12 117.68(15)
O7 C13 C14 122.41(15)
C12 C13 C14 119.92(15)
C15 C14 C13 119.85(16)
C14 C15 C10 120.78(16)
C1 N1 N2 110.02(13)
C2 N2 N1 116.61(13)
C2 N2 Mo 127.25(11)
N1 N2 Mo 115.38(9)
C6 N3 C5 119.17(14)
C1 O1 Mo 120.16(10)
C7 O2 Mo 132.62(10)
C16 O6 Mo 121.74(11)
O4 Mo O5 105.28(6)
O4 Mo O2 99.79(5)
O5 Mo O2 105.80(5)
O4 Mo O1 95.64(5)
O5 Mo O1 97.72(5)
O2 Mo O1 147.16(5)
O4 Mo N2 89.17(5)
O5 Mo N2 162.87(5)
O2 Mo N2 80.12(5)
O1 Mo N2 71.26(5)
O4 Mo O6 170.50(5)
O5 Mo O6 83.50(5)
O2 Mo O6 80.91(5)
O1 Mo O6 79.32(5)
N2 Mo O6 81.60(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.3088(19)
C1 N1 1.309(2)
C1 C10 1.467(2)
C2 N2 1.287(2)
C2 C3 1.453(2)
C3 C7 1.404(2)
C3 C4 1.417(2)
C4 C5 1.373(2)
C4 C9 1.509(2)
C5 N3 1.350(2)
C6 N3 1.328(2)
C6 C7 1.416(2)
C6 C8 1.495(2)
C7 O2 1.3387(19)
C9 O3 1.424(2)
C10 C11 1.398(2)
C10 C15 1.401(2)
C11 C12 1.382(2)
C12 C13 1.392(2)
C13 O7 1.360(2)
C13 C14 1.396(2)
C14 C15 1.379(2)
C16 O6 1.439(2)
C17 O8 1.428(2)
N1 N2 1.3918(18)
N2 Mo 2.2585(13)
O1 Mo 2.0378(12)
O2 Mo 1.9325(12)
O4 Mo 1.6987(12)
O5 Mo 1.7015(11)
O6 Mo 2.2659(12)
