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_7217760
_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            'C15 H16 Mo N4 O6'
_chemical_formula_weight         444.26
_chemical_name_systematic
;
methanol(pyridoxal-isonicotinoyl
-hydrazone-
N,O,O)-dioxa-molybdenum(VI)
;
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                99.59(5)
_cell_angle_beta                 99.50(6)
_cell_angle_gamma                93.09(6)
_cell_formula_units_Z            2
_cell_length_a                   7.700(6)
_cell_length_b                   8.392(5)
_cell_length_c                   13.071(7)
_cell_measurement_temperature    295(2)
_cell_volume                     818.5(9)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.985
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15649
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.983
_diffrn_reflns_theta_min         3.756
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84255
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       needle
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3523
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.3703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3097
_reflns_number_total             3523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra08179j2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        818.5(10)
_cod_database_code               7217760
_shelxl_version_number           2013-4
_shelx_res_checksum              84461