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_7217758
_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            'C23 H34 Mo6 N4 O25'
_chemical_formula_weight         1342.18
_chemical_name_systematic
;
 pyridoxal-isonicotinoyl-hydrazone (\mU~eq~6-oxo)
-dodecakis(\mU~eq~2-oxo)-hexa(oxomolybdenum) 
acetone solvate (1/3)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 109.882(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5047(2)
_cell_length_b                   18.6297(3)
_cell_length_c                   10.7312(2)
_cell_measurement_reflns_used    14830
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      32.6140
_cell_measurement_theta_min      4.1175
_cell_volume                     1974.91(7)
_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 0.994
_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  0.0156
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16634
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         4.184
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.257
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 3035 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.003(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7685
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0354P)^2^+0.6819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.820
_reflns_Friedel_fraction_max     0.782
_reflns_number_gt                7199
_reflns_number_total             7685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra08179j2.cif
_cod_data_source_block           shelx
_cod_database_code               7217758
_shelxl_version_number           2013-4
_shelx_res_checksum              60224