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_7217757
_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 H17 Mo4 N4 O14.5'
_chemical_formula_weight         893.10
_chemical_name_systematic
;
bis(cis-(NCsp^3^'-((3-oxy)-5-(hydroxymethyl)-2-methylpyridin-4-yl)methylene)benzhydrazonato-dioxo-molybdenum(VI)) (\mU~eq~6-oxo)-dodecakis(\mU~eq~2-oxo)-hexa(oxomolybdenum) acetonitrile solvate (1/2)
;
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.04016(12)
_cell_length_b                   16.04016(12)
_cell_length_c                   17.79763(16)
_cell_measurement_reflns_used    17583
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.0608
_cell_measurement_theta_min      4.2644
_cell_volume                     3965.61(6)
_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 0.991
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur,detector Sapphire3'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22953
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         4.273
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87676
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_description       needle
_exptl_crystal_F_000             2586
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 2721 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.038(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6372
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+1.5879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0456
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6167
_reflns_number_total             6372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra08179j2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3965.61(7)
_cod_original_formula_sum        'C17 H17 Mo4 N4 O14.50'
_cod_database_code               7217757
_shelxl_version_number           2013-4
_shelx_res_checksum              27659