Towards a global greener process: from solvent-less synthesis of molybdenum(vi) ONO Schiff base complexes to catalyzed olefin epoxidation under organic-solvent-free conditions
Cindrić, Marina; Pavlović, Gordana; Katava, Robert; Agustin, Dominique; New J. Chem. 41 (2017) 594–; doi:10.1039/C6NJ03174A

data_1544799
_publ_section_title
;
 Towards a global greener process: from solvent-less synthesis of
 molybdenum(vi) ONO Schiff base complexes to catalyzed olefin epoxidation
 under organic-solvent-free conditions
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              594
_journal_paper_doi               10.1039/C6NJ03174A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C19 H17 Mo N O5, C H4 O'
_chemical_formula_sum            'C20 H21 Mo N O6'
_chemical_formula_weight         467.32
_chemical_name_systematic
cis-dioxo(2-(N-(2-oxonapht-1-yl)methylamino)-5-methylphenolato-N,O,O')-(methanol)-molybdenum(VI)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-04 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.268(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9476(13)
_cell_length_b                   14.9809(14)
_cell_length_c                   16.765(3)
_cell_measurement_reflns_used    1829
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.1157
_cell_measurement_theta_min      4.2398
_cell_volume                     1984.1(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'MERCURY 3.7. (CCDC, 2015)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7285
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.495
_diffrn_reflns_theta_min         4.260
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4084
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0358P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2347
_reflns_number_total             4084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03174a2.cif
_cod_data_source_block           9_2608
_cod_depositor_comments
'Adding full bibliography for 1544795--1544799.cif.'
_cod_database_code               1544799
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              81960