#------------------------------------------------------------------------------
#$Date: 2021-07-01 11:23:50 +0300 (Thu, 01 Jul 2021) $
#$Revision: 266860 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/38/1563833.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1563833
loop_
_publ_author_name
'Romanowski, Grzegorz'
'Kira, Jaromir'
'Wera, Michał'
_publ_section_title
;
 Synthesis, structure, spectroscopic characterization and catalytic
 activity of chiral dioxidomolybdenum(VI) Schiff base complexes derived
 from R(−)-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/[σ²(Fo²)+(0.0481P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.73036(4) 0.20277(3) 0.13237(4) 0.03196(14) Uani 1 1 d . . . . .
O1 O 0.8639(4) 0.1271(4) 0.0874(3) 0.0394(9) Uani 1 1 d . . . . .
N1 N 0.8426(4) 0.1116(4) 0.3034(3) 0.0297(10) Uani 1 1 d . . . . .
C1 C 0.9365(5) 0.0282(6) 0.1197(4) 0.0314(12) Uani 1 1 d . . . . .
O2 O 0.6697(4) 0.2805(4) 0.2458(3) 0.0399(9) Uani 1 1 d . . . . .
C2 C 0.9841(6) -0.0266(7) 0.0416(5) 0.0444(16) Uani 1 1 d . . . . .
H2A H 0.9613 0.0045 -0.0331 0.053 Uiso 1 1 calc R U . . .
Mo2 Mo 0.77863(4) 0.63452(4) 0.35964(4) 0.03424(15) Uani 1 1 d . . . . .
O3 O 0.6791(4) 0.3151(4) 0.0306(3) 0.0461(10) Uani 1 1 d . . . . .
C3 C 1.0636(6) -0.1253(7) 0.0714(5) 0.0465(16) Uani 1 1 d . . . . .
H3B H 1.0936 -0.1598 0.0166 0.056 Uiso 1 1 calc R U . . .
O4 O 0.6222(4) 0.0892(4) 0.0896(3) 0.0489(11) Uani 1 1 d . . . . .
C4 C 1.1007(5) -0.1753(6) 0.1816(5) 0.0367(13) Uani 1 1 d . . . . .
O5 O 0.9034(4) 0.3393(4) 0.2173(4) 0.0444(10) Uani 1 1 d . . . . .
H5B H 0.8780 0.4204 0.2155 0.053 Uiso 1 1 calc R U . . .
C5 C 1.0523(6) -0.1229(6) 0.2591(5) 0.0329(13) Uani 1 1 d . . . . .
H5A H 1.0749 -0.1558 0.3331 0.039 Uiso 1 1 calc R U . . .
C6 C 0.9700(5) -0.0216(5) 0.2312(4) 0.0281(12) Uani 1 1 d . . . . .
C7 C 0.9257(5) 0.0291(5) 0.3199(4) 0.0300(12) Uani 1 1 d . . . . .
H7A H 0.9616 -0.0017 0.3946 0.036 Uiso 1 1 calc R U . . .
C8 C 0.8105(5) 0.1621(5) 0.4025(5) 0.0379(13) Uani 1 1 d . . . . .
H8A H 0.8699 0.2286 0.4376 0.045 Uiso 1 1 calc R U . . .
C9 C 0.6764(5) 0.2157(7) 0.3464(5) 0.0446(14) Uani 1 1 d . . . . .
H9A H 0.6138 0.1504 0.3268 0.054 Uiso 1 1 calc R U . . .
H9B H 0.6572 0.2699 0.4005 0.054 Uiso 1 1 calc R U . . .
C10 C 0.8155(7) 0.0700(8) 0.4950(5) 0.0556(18) Uani 1 1 d . . . . .
H10A H 0.9028 0.0555 0.5422 0.083 Uiso 1 1 calc R U . . .
H10B H 0.7772 -0.0050 0.4594 0.083 Uiso 1 1 calc R U . . .
H10C H 0.7697 0.1010 0.5424 0.083 Uiso 1 1 calc R U . . .
C11 C 1.1890(6) -0.2833(7) 0.2134(5) 0.0538(17) Uani 1 1 d . . . . .
H11A H 1.2680 -0.2596 0.2716 0.081 Uiso 1 1 calc R U . . .
H11B H 1.2053 -0.3118 0.1461 0.081 Uiso 1 1 calc R U . . .
H11C H 1.1501 -0.3473 0.2430 0.081 Uiso 1 1 calc R U . . .
C12 C 1.0361(6) 0.3232(7) 0.2696(7) 0.058(2) Uani 1 1 d . . . . .
H12A H 1.0799 0.3876 0.2457 0.087 Uiso 1 1 calc R U . . .
H12B H 1.0602 0.2460 0.2464 0.087 Uiso 1 1 calc R U . . .
H12C H 1.0587 0.3249 0.3522 0.087 Uiso 1 1 calc R U . . .
O21 O 0.6478(3) 0.7053(5) 0.4101(3) 0.0400(9) Uani 1 1 d . . . . .
N21 N 0.6807(4) 0.7510(4) 0.2011(4) 0.0293(10) Uani 1 1 d . . . . .
C21 C 0.5673(5) 0.8018(6) 0.3792(4) 0.0346(13) Uani 1 1 d . . . . .
O22 O 0.8317(4) 0.5650(4) 0.2375(3) 0.0442(10) Uani 1 1 d . . . . .
C22 C 0.5122(6) 0.8428(7) 0.4583(5) 0.0455(16) Uani 1 1 d . . . . .
H22A H 0.5330 0.8052 0.5302 0.055 Uiso 1 1 calc R U . . .
O23 O 0.8206(4) 0.5115(5) 0.4492(4) 0.0546(12) Uani 1 1 d . . . . .
C23 C 0.4268(6) 0.9390(6) 0.4308(5) 0.0449(16) Uani 1 1 d . . . . .
H23B H 0.3929 0.9663 0.4857 0.054 Uiso 1 1 calc R U . . .
O24 O 0.8957(4) 0.7394(5) 0.4159(4) 0.0540(13) Uani 1 1 d . . . . .
C24 C 0.3903(5) 0.9956(6) 0.3242(5) 0.0372(13) Uani 1 1 d . . . . .
O25 O 0.6014(4) 0.5117(4) 0.2579(4) 0.0517(11) Uani 1 1 d . . . . .
H25B H 0.6238 0.4386 0.2315 0.062 Uiso 1 1 calc R U . . .
C25 C 0.4443(6) 0.9530(6) 0.2454(5) 0.0348(14) Uani 1 1 d . . . . .
H25A H 0.4207 0.9892 0.1727 0.042 Uiso 1 1 calc R U . . .
C26 C 0.5324(5) 0.8583(5) 0.2712(4) 0.0309(13) Uani 1 1 d . . . . .
C27 C 0.5896(5) 0.8274(5) 0.1847(5) 0.0307(12) Uani 1 1 d . . . . .
H27A H 0.5578 0.8657 0.1130 0.037 Uiso 1 1 calc R U . . .
C28 C 0.7406(5) 0.7328(5) 0.1127(4) 0.0342(12) Uani 1 1 d . . . . .
H28A H 0.8208 0.7789 0.1379 0.041 Uiso 1 1 calc R U . . .
C29 C 0.7748(6) 0.6016(6) 0.1189(5) 0.0471(16) Uani 1 1 d . . . . .
H29A H 0.6988 0.5533 0.0817 0.056 Uiso 1 1 calc R U . . .
H29B H 0.8343 0.5875 0.0784 0.056 Uiso 1 1 calc R U . . .
C30 C 0.6654(6) 0.7740(7) -0.0096(4) 0.0507(17) Uani 1 1 d . . . . .
H30A H 0.6490 0.8600 -0.0097 0.076 Uiso 1 1 calc R U . . .
H30B H 0.5859 0.7306 -0.0374 0.076 Uiso 1 1 calc R U . . .
H30C H 0.7138 0.7574 -0.0591 0.076 Uiso 1 1 calc R U . . .
C31 C 0.2963(6) 1.1013(6) 0.2948(5) 0.0464(16) Uani 1 1 d . . . . .
H31A H 0.2589 1.1092 0.3539 0.070 Uiso 1 1 calc R U . . .
H31B H 0.2304 1.0860 0.2217 0.070 Uiso 1 1 calc R U . . .
H31C H 0.3402 1.1753 0.2901 0.070 Uiso 1 1 calc R U . . .
C32 C 0.4696(7) 0.5267(8) 0.2293(7) 0.066(2) Uani 1 1 d . . . . .
H32A H 0.4290 0.4482 0.2176 0.099 Uiso 1 1 calc R U . . .
H32B H 0.4367 0.5739 0.1596 0.099 Uiso 1 1 calc R U . . .
H32C H 0.4526 0.5684 0.2911 0.099 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O4 Mo1 O3 106.2(2) . .
O4 Mo1 O2 99.14(19) . .
O3 Mo1 O2 95.72(19) . .
O4 Mo1 O1 97.6(2) . .
O3 Mo1 O1 101.20(19) . .
O2 Mo1 O1 151.76(16) . .
O4 Mo1 N1 94.11(18) . .
O3 Mo1 N1 158.92(19) . .
O2 Mo1 N1 75.24(16) . .
O1 Mo1 N1 81.04(14) . .
O4 Mo1 O5 170.28(19) . .
O3 Mo1 O5 83.41(18) . .
O2 Mo1 O5 80.78(15) . .
O1 Mo1 O5 78.90(17) . .
N1 Mo1 O5 76.42(15) . .
C1 O1 Mo1 135.3(3) . .
C7 N1 C8 120.3(4) . .
C7 N1 Mo1 127.1(3) . .
C8 N1 Mo1 112.5(3) . .
O1 C1 C2 119.1(5) . .
O1 C1 C6 122.6(5) . .
C2 C1 C6 118.3(5) . .
C9 O2 Mo1 119.0(4) . .
C3 C2 C1 121.7(5) . .
O24 Mo2 O23 105.7(2) . .
O24 Mo2 O21 99.1(2) . .
O23 Mo2 O21 100.4(2) . .
O24 Mo2 O22 100.5(2) . .
O23 Mo2 O22 95.8(2) . .
O21 Mo2 O22 150.11(15) . .
O24 Mo2 N21 92.58(19) . .
O23 Mo2 N21 160.9(2) . .
O21 Mo2 N21 81.79(15) . .
O22 Mo2 N21 75.03(16) . .
O24 Mo2 O25 170.87(19) . .
O23 Mo2 O25 83.4(2) . .
O21 Mo2 O25 79.16(18) . .
O22 Mo2 O25 77.89(17) . .
N21 Mo2 O25 78.32(16) . .
C2 C3 C4 121.5(5) . .
C5 C4 C3 117.2(6) . .
C5 C4 C11 121.9(5) . .
C3 C4 C11 120.9(5) . .
C12 O5 Mo1 133.5(4) . .
C4 C5 C6 122.7(5) . .
C1 C6 C5 118.5(5) . .
C1 C6 C7 122.7(5) . .
C5 C6 C7 118.7(5) . .
N1 C7 C6 125.0(5) . .
N1 C8 C10 114.4(5) . .
N1 C8 C9 104.2(4) . .
C10 C8 C9 111.9(5) . .
O2 C9 C8 109.7(4) . .
C21 O21 Mo2 136.4(3) . .
C27 N21 C28 120.7(4) . .
C27 N21 Mo2 128.7(4) . .
C28 N21 Mo2 110.6(3) . .
O21 C21 C22 117.8(5) . .
O21 C21 C26 123.7(4) . .
C22 C21 C26 118.5(5) . .
C29 O22 Mo2 122.0(3) . .
C23 C22 C21 120.5(6) . .
C24 C23 C22 121.9(5) . .
C23 C24 C25 117.2(5) . .
C23 C24 C31 121.5(5) . .
C25 C24 C31 121.3(5) . .
C32 O25 Mo2 133.0(5) . .
C24 C25 C26 122.4(5) . .
C25 C26 C21 119.5(5) . .
C25 C26 C27 117.4(5) . .
C21 C26 C27 123.0(5) . .
N21 C27 C26 124.2(5) . .
N21 C28 C29 105.5(4) . .
N21 C28 C30 117.1(4) . .
C29 C28 C30 112.6(5) . .
O22 C29 C28 109.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O4 1.686(4) .
Mo1 O3 1.708(4) .
Mo1 O2 1.944(4) .
Mo1 O1 1.944(3) .
Mo1 N1 2.276(4) .
Mo1 O5 2.380(4) .
O1 C1 1.329(7) .
N1 C7 1.260(7) .
N1 C8 1.490(6) .
C1 C2 1.385(8) .
C1 C6 1.402(7) .
O2 C9 1.407(7) .
C2 C3 1.366(9) .
Mo2 O24 1.698(4) .
Mo2 O23 1.702(4) .
Mo2 O21 1.934(4) .
Mo2 O22 1.950(4) .
Mo2 N21 2.272(4) .
Mo2 O25 2.363(4) .
C3 C4 1.387(8) .
C4 C5 1.373(8) .
C4 C11 1.502(9) .
O5 C12 1.408(8) .
C5 C6 1.405(8) .
C6 C7 1.455(7) .
C8 C10 1.508(9) .
C8 C9 1.533(8) .
O21 C21 1.354(7) .
N21 C27 1.278(7) .
N21 C28 1.474(6) .
C21 C22 1.393(7) .
C21 C26 1.394(7) .
O22 C29 1.434(7) .
C22 C23 1.382(9) .
C23 C24 1.380(8) .
C24 C25 1.386(8) .
C24 C31 1.520(8) .
O25 C32 1.399(8) .
C25 C26 1.389(8) .
C26 C27 1.456(7) .
C28 C29 1.482(8) .
C28 C30 1.518(7) .
