Synthesis, structure, spectroscopic characterization and catalytic activity of chiral dioxidomolybdenum(VI) Schiff base complexes derived from R(−)-2-amino-1-propanol
Romanowski, Grzegorz; Kira, Jaromir; Wera, Michał; Inorganica Chimica Acta 483 (2018) 156–164; doi:10.1016/j.ica.2018.08.022

data_1563833
_publ_section_title
;
 Synthesis, structure, spectroscopic characterization and catalytic
 activity of chiral dioxidomolybdenum(VI) Schiff base complexes derived
 from R(&#x2212;)-2-amino-1-propanol
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              156
_journal_page_last               164
_journal_paper_doi               10.1016/j.ica.2018.08.022
_journal_volume                  483
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_sum            'C12 H17 Mo N O5'
_chemical_formula_weight         351.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.141(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1573(6)
_cell_length_b                   10.9549(4)
_cell_length_c                   12.3044(6)
_cell_measurement_reflns_used    10472
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.39
_cell_volume                     1411.96(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.4002
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       /w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9728
_diffrn_reflns_point_group_measured_fraction_full 0.813
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        25.998
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         3.391
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.99
_exptl_crystal_size_mid          0.72
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 1465 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4520
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0481P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.545
_reflns_Friedel_fraction_full    0.607
_reflns_Friedel_fraction_max     0.607
_reflns_number_gt                4282
_reflns_number_total             4520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-483-156.cif
_cod_data_source_block           I
_cod_original_cell_volume        1411.97(13)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1563833
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              99899
_shelx_hkl_checksum              51849