Synthesis and X-ray crystal structure of a Molybdenum(VI) Schiff base complex: Design of a new catalytic system for sustainable olefin epoxidation
Mahmoudi, Hamed; Bagherzadeh, Mojtaba; Ataie, Saeed; Kia, Reza; Heydar Moravej, Seyed; Zare, Maryam; Raithby, Paul R.; Ferlin, Francesco; Vaccaro, Luigi; Inorganica Chimica Acta 511 (2020) 119775–; doi:10.1016/j.ica.2020.119775

data_1564160
_publ_section_title
;
 Synthesis and X-ray crystal structure of a Molybdenum(VI) Schiff base
 complex: Design of a new catalytic system for sustainable olefin
 epoxidation
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119775
_journal_paper_doi               10.1016/j.ica.2020.119775
_journal_volume                  511
_journal_year                    2020
_chemical_formula_moiety         'C32 H27 Mo N O5 P, C32 H25 Cl Mo N O4 P, Cl'
_chemical_formula_sum            'C64 H52 Cl2 Mo2 N2 O9 P2'
_chemical_formula_weight         1317.79
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.2043(3)
_cell_length_b                   12.2043(3)
_cell_length_c                   76.2069(17)
_cell_measurement_reflns_used    5625
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.0170
_cell_measurement_theta_min      4.1490
_cell_volume                     9829.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    xp
_computing_publication_material  shelxtl
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    xt
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.2300
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       93
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            30889
_diffrn_reflns_point_group_measured_fraction_full 0.702
_diffrn_reflns_point_group_measured_fraction_max 0.682
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.091
_diffrn_reflns_theta_min         4.183
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             4020
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         8782
_refine_ls_number_restraints     566
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0609P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.367
_reflns_Friedel_fraction_full    0.399
_reflns_Friedel_fraction_max     0.369
_reflns_number_gt                7390
_reflns_number_total             8782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-511-119775.cif
_cod_data_source_block           complex
_cod_original_cell_volume        9829.9(5)
_cod_database_code               1564160
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.575
_shelx_estimated_absorpt_t_max   0.796
_shelx_res_checksum              39596
_shelx_hkl_checksum              29977
_shelx_fab_checksum              30469