Pyridoxal hydrazonato molybdenum(VI) complexes: Assembly, Structure and Epoxidation (Pre)Catalyst testing under solvent-free conditions
Pisk, Jana; Prugovečki, Biserka; Matković-Čalogović, Dubravka; Jednačak, Tomislav; Novak, Predrag; Agustin, Dominique; Vrdoljak, Visnja; RSC Advances  (2014) –; doi:10.1039/C4RA08179J

data_7217762
_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/[\s^2^(Fo^2^)+(0.0301P)^2^+0.1520P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            c4ra08179j2.cif
_cod_data_source_block           shelx
_cod_database_code               7217762
_shelxl_version_number           2013-4
_shelx_res_checksum              4054