# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_f
_database_code_depnum_ccdc_archive 'CCDC 1941205'
loop_
_audit_author_name
_audit_author_address
'Sudeshna Chatterjee'
;THE UNIVERSITY OF BURDWAN
India
;
_audit_update_record             
;
2020-02-26 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H24 Mo N3 O5'
_chemical_formula_weight         482.36

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'
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   13.7533(17)
_cell_length_b                   20.0569(10)
_cell_length_c                   7.505(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2070.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    440
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      25.30

_exptl_crystal_description       Block
_exptl_crystal_colour            Bronze
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_F_000             988
_exptl_transmission_factor_min   0.5604
_exptl_transmission_factor_max   0.7452
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.670
_shelx_estimated_absorpt_T_min   0.886
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12471
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         1.795
_diffrn_reflns_theta_max         25.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.785
_diffrn_reflns_point_group_measured_fraction_full 0.788
_reflns_number_total             3787
_reflns_number_gt                2267
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.454
_reflns_Friedel_fraction_max     0.535
_reflns_Friedel_fraction_full    0.539

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1364P)²+24.0001P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 631 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.08(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2976
_refine_ls_number_parameters     266
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0843
_refine_ls_wR_factor_ref         0.2984
_refine_ls_wR_factor_gt          0.2843
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_restrained_S_all      1.280
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mo Mo 0.26954(11) 0.56330(8) 0.5133(4) 0.0294(6) Uani 1 1 d . . . . .
O1 O 0.2893(9) 0.4641(6) 0.495(3) 0.032(4) Uani 1 1 d . . . . .
O2 O 0.3226(11) 0.6513(7) 0.544(3) 0.035(5) Uani 1 1 d . . . . .
O3 O 0.3652(11) 0.5444(7) 0.773(2) 0.032(4) Uani 1 1 d . . . . .
O4 O 0.2196(13) 0.5745(8) 0.310(3) 0.044(5) Uani 1 1 d . . . . .
O5 O 0.1732(12) 0.5608(8) 0.661(3) 0.033(4) Uani 1 1 d . . . . .
N1 N 0.4401(12) 0.4759(8) 0.368(3) 0.028(4) Uani 1 1 d . . . . .
N2 N 0.4162(14) 0.5438(10) 0.408(3) 0.037(5) Uani 1 1 d . . . . .
N3 N 0.4142(15) 0.8646(9) 0.324(3) 0.037(5) Uani 1 1 d . . . . .
C1 C 0.3666(15) 0.4417(12) 0.419(3) 0.031(5) Uani 1 1 d . . . . .
C2 C 0.3671(15) 0.3679(11) 0.381(4) 0.032(5) Uani 1 1 d . . . . .
C3 C 0.2868(19) 0.3297(12) 0.434(3) 0.037(6) Uani 1 1 d . . . . .
H3 H 0.2342 0.3513 0.4927 0.045 Uiso 1 1 calc R U . . .
C4 C 0.2811(15) 0.2617(11) 0.405(3) 0.029(5) Uani 1 1 d . . . . .
C5 C 0.3573(18) 0.2316(12) 0.319(3) 0.038(6) Uani 1 1 d . . . . .
H5 H 0.3537 0.1849 0.2988 0.045 Uiso 1 1 calc R U . . .
C6 C 0.437(2) 0.2641(12) 0.262(4) 0.046(8) Uani 1 1 d . . . . .
H6 H 0.4872 0.2410 0.2006 0.055 Uiso 1 1 calc R U . . .
C7 C 0.4449(19) 0.3341(11) 0.295(3) 0.037(6) Uani 1 1 d . . . . .
H7 H 0.5015 0.3578 0.2593 0.044 Uiso 1 1 calc R U . . .
C8 C 0.1915(18) 0.2197(12) 0.466(4) 0.046(9) Uani 1 1 d . . . . .
H8A H 0.1684 0.1923 0.3668 0.069 Uiso 1 1 calc R U . . .
H8B H 0.1394 0.2498 0.5050 0.069 Uiso 1 1 calc R U . . .
H8C H 0.2105 0.1908 0.5656 0.069 Uiso 1 1 calc R U . . .
C9 C 0.4803(14) 0.5899(11) 0.352(4) 0.028(5) Uani 1 1 d . . . . .
H9 H 0.5392 0.5743 0.3013 0.033 Uiso 1 1 calc R U . . .
C10 C 0.4679(15) 0.6583(12) 0.364(3) 0.030(5) Uani 1 1 d . . . . .
C11 C 0.3833(16) 0.6889(11) 0.446(3) 0.030(5) Uani 1 1 d . . . . .
C12 C 0.3675(16) 0.7593(10) 0.437(3) 0.028(5) Uani 1 1 d . . . . .
H12 H 0.3127 0.7793 0.4932 0.034 Uiso 1 1 calc R U . . .
C13 C 0.435(2) 0.7975(14) 0.344(4) 0.043(6) Uani 1 1 d . . . . .
C14 C 0.5168(19) 0.7707(12) 0.271(3) 0.035(6) Uani 1 1 d . . . . .
H14 H 0.5627 0.7992 0.2144 0.042 Uiso 1 1 calc R U . . .
C15 C 0.5333(16) 0.7053(12) 0.277(3) 0.031(5) Uani 1 1 d . . . . .
H15 H 0.5906 0.6885 0.2225 0.037 Uiso 1 1 calc R U . . .
C16 C 0.4871(17) 0.9136(13) 0.243(4) 0.040(7) Uani 1 1 d . . . . .
H16A H 0.4738 0.9593 0.2865 0.049 Uiso 1 1 calc R U . . .
H16B H 0.5541 0.9012 0.2778 0.049 Uiso 1 1 calc R U . . .
C17 C 0.4772(17) 0.9114(12) 0.043(4) 0.042(8) Uani 1 1 d . . . . .
H17A H 0.4818 0.8651 0.0023 0.063 Uiso 1 1 calc R U . . .
H17B H 0.5293 0.9377 -0.0114 0.063 Uiso 1 1 calc R U . . .
H17C H 0.4140 0.9299 0.0084 0.063 Uiso 1 1 calc R U . . .
C18 C 0.331(2) 0.8983(15) 0.413(5) 0.047(8) Uani 1 1 d . . . . .
H18A H 0.2738 0.8685 0.4115 0.056 Uiso 1 1 calc R U . . .
H18B H 0.3142 0.9393 0.3465 0.056 Uiso 1 1 calc R U . . .
C19 C 0.357(3) 0.9162(17) 0.606(5) 0.054(9) Uani 1 1 d . . . . .
H19A H 0.3738 0.8756 0.6709 0.081 Uiso 1 1 calc R U . . .
H19B H 0.3004 0.9374 0.6624 0.081 Uiso 1 1 calc R U . . .
H19C H 0.4118 0.9470 0.6066 0.081 Uiso 1 1 calc R U . . .
C20 C 0.3352(19) 0.5412(14) 0.952(4) 0.045(7) Uani 1 1 d . . . . .
H20A H 0.2705 0.5612 0.9634 0.068 Uiso 1 1 calc R U . . .
H20B H 0.3814 0.5657 1.0267 0.068 Uiso 1 1 calc R U . . .
H20C H 0.3328 0.4945 0.9901 0.068 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo O4 1.69(2) . ?
Mo O5 1.727(16) . ?
Mo O2 1.925(15) . ?
Mo O1 2.012(13) . ?
Mo N2 2.20(2) . ?
Mo O3 2.385(17) . ?
O1 C1 1.29(3) . ?
O2 C11 1.34(3) . ?
O3 C20 1.40(3) . ?
N1 C1 1.28(3) . ?
N1 N2 1.43(3) . ?
N2 C9 1.34(3) . ?
N3 C13 1.38(3) . ?
N3 C18 1.49(4) . ?
N3 C16 1.53(3) . ?
C1 C2 1.51(3) . ?
C2 C3 1.40(3) . ?
C2 C7 1.42(3) . ?
C3 C4 1.38(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.37(3) . ?
C4 C8 1.56(3) . ?
C5 C6 1.35(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.43(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.38(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.45(3) . ?
C10 C15 1.46(3) . ?
C11 C12 1.43(3) . ?
C12 C13 1.39(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.37(4) . ?
C14 C15 1.33(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.50(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.53(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

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
_geom_angle_publ_flag
O4 Mo O5 105.7(10) . . ?
O4 Mo O2 98.2(8) . . ?
O5 Mo O2 103.9(7) . . ?
O4 Mo O1 97.2(9) . . ?
O5 Mo O1 96.8(7) . . ?
O2 Mo O1 149.8(6) . . ?
O4 Mo N2 94.1(9) . . ?
O5 Mo N2 158.2(9) . . ?
O2 Mo N2 81.9(7) . . ?
O1 Mo N2 71.1(7) . . ?
O4 Mo O3 170.3(8) . . ?
O5 Mo O3 83.9(8) . . ?
O2 Mo O3 80.7(6) . . ?
O1 Mo O3 79.8(8) . . ?
N2 Mo O3 76.2(7) . . ?
C1 O1 Mo 119.1(14) . . ?
C11 O2 Mo 133.1(16) . . ?
C20 O3 Mo 128.8(14) . . ?
C1 N1 N2 105.5(18) . . ?
C9 N2 N1 116(2) . . ?
C9 N2 Mo 126.2(17) . . ?
N1 N2 Mo 117.0(12) . . ?
C13 N3 C18 123(2) . . ?
C13 N3 C16 122(2) . . ?
C18 N3 C16 113(2) . . ?
N1 C1 O1 127(2) . . ?
N1 C1 C2 118(2) . . ?
O1 C1 C2 115.5(19) . . ?
C3 C2 C7 118(2) . . ?
C3 C2 C1 119(2) . . ?
C7 C2 C1 124(2) . . ?
C4 C3 C2 122(2) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C5 C4 C3 118(2) . . ?
C5 C4 C8 120(2) . . ?
C3 C4 C8 122(2) . . ?
C6 C5 C4 124(2) . . ?
C6 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C5 C6 C7 119(2) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C2 C7 C6 119(2) . . ?
C2 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 126(2) . . ?
N2 C9 H9 117.2 . . ?
C10 C9 H9 117.2 . . ?
C9 C10 C11 123(2) . . ?
C9 C10 C15 123(2) . . ?
C11 C10 C15 114(2) . . ?
O2 C11 C12 119(2) . . ?
O2 C11 C10 120(2) . . ?
C12 C11 C10 121(2) . . ?
C13 C12 C11 118(2) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
C14 C13 N3 120(2) . . ?
C14 C13 C12 123(3) . . ?
N3 C13 C12 117(2) . . ?
C15 C14 C13 121(3) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C10 123(2) . . ?
C14 C15 H15 118.4 . . ?
C10 C15 H15 118.4 . . ?
C17 C16 N3 109(2) . . ?
C17 C16 H16A 110.0 . . ?
N3 C16 H16A 110.0 . . ?
C17 C16 H16B 110.0 . . ?
N3 C16 H16B 110.0 . . ?
H16A C16 H16B 108.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 111(3) . . ?
N3 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
N3 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_refine_diff_density_max         1.506
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.218

_shelxl_version_number           2013-4

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ddvf163
_database_code_depnum_ccdc_archive 'CCDC 1919499'
loop_
_audit_author_name
_audit_author_address
'Sudeshna Chatterjee'
;THE UNIVERSITY OF BURDWAN
India
;
_audit_update_record             
;
2020-02-26 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;
_audit_creation_date             2017-06-09
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_chemical_formula_moiety         'C20 H17 Mo N2 O5'
_chemical_formula_sum            'C20 H17 Mo N2 O5'
_chemical_formula_weight         461.30
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Mo -1.68402 0.70339 3.70250 17.23560 12.88760 3.74290 0.27720 1.09580 11.00400
61.65840 4.38749980927
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   7.7042(4)
_cell_length_b                   16.2189(8)
_cell_length_c                   14.9336(7)
_cell_angle_alpha                90
_cell_angle_beta                 102.051(2)
_cell_angle_gamma                90
_cell_volume                     1824.89(16)
_cell_formula_units_Z            4
_exptl_absorpt_coefficient_mu    0.754
_exptl_crystal_density_diffrn    1.6789
_exptl_crystal_F_000             925.5323
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48300
_diffrn_reflns_theta_full        29.1845
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         2.51
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4175
_reflns_number_total             4945
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.8456
_refine_diff_density_min         -0.7718
_refine_diff_density_rms         0.0993
_refine_ls_d_res_high            0.7288
_refine_ls_d_res_low             8.1095
_refine_ls_goodness_of_fit_ref   1.0739
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4945
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0264
_refine_ls_restrained_S_all      1.0739
_refine_ls_shift/su_max          0.0127
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0288P)²+1.9251P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0703
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C20(H20a,H20b,H20c)
;
_atom_sites_solution_primary     direct
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_refinement_flags_posn
Mo Mo 0.69822(2) 0.696079(10) 0.497503(11) 0.01903(6) Uani 1.000000 .
O1 O 0.66375(19) 0.64863(8) 0.61686(9) 0.0222(3) Uani 1.000000 .
O2 O 0.6898(2) 0.68344(8) 0.36825(10) 0.0252(3) Uani 1.000000 .
O3 O 0.5870(2) 0.78609(9) 0.50356(10) 0.0275(3) Uani 1.000000 .
O4 O 0.9165(2) 0.71862(10) 0.53311(11) 0.0307(3) Uani 1.000000 .
O5 O 0.40801(19) 0.64454(9) 0.45631(10) 0.0256(3) Uani 1.000000 .
N1 N 0.7002(2) 0.51653(10) 0.56792(10) 0.0185(3) Uani 1.000000 .
N2 N 0.7274(2) 0.55975(10) 0.49076(10) 0.0174(3) Uani 1.000000 .
C1 C 0.6736(2) 0.56886(11) 0.63060(13) 0.0182(3) Uani 1.000000 .
C2 C 0.6487(2) 0.53816(12) 0.71986(12) 0.0192(4) Uani 1.000000 .
C3 C 0.5833(3) 0.59065(13) 0.77915(14) 0.0249(4) Uani 1.000000 .
H3 H 0.5563(3) 0.64650(13) 0.76275(14) 0.0298(5) Uiso 1.000000 R
C4 C 0.5581(3) 0.56029(15) 0.86213(15) 0.0314(5) Uani 1.000000 .
H4 H 0.5137(3) 0.59565(15) 0.90287(15) 0.0377(6) Uiso 1.000000 R
C5 C 0.5969(3) 0.47894(16) 0.88636(14) 0.0303(5) Uani 1.000000 .
H5 H 0.5782(3) 0.45918(16) 0.94347(14) 0.0363(6) Uiso 1.000000 R
C6 C 0.6629(3) 0.42563(14) 0.82854(14) 0.0263(4) Uani 1.000000 .
C7 C 0.6897(3) 0.45676(13) 0.74571(13) 0.0208(4) Uani 1.000000 .
H7 H 0.7372(3) 0.42170(13) 0.70583(13) 0.0249(4) Uiso 1.000000 R
C8 C 0.7058(4) 0.33737(17) 0.85474(18) 0.0402(6) Uani 1.000000 .
H8a H 0.698(3) 0.3041(3) 0.79926(18) 0.0604(9) Uiso 1.000000 GR
H8b H 0.8265(10) 0.3339(2) 0.8920(12) 0.0604(9) Uiso 1.000000 GR
H8c H 0.6213(17) 0.3166(4) 0.8901(12) 0.0604(9) Uiso 1.000000 GR
C9 C 0.7652(2) 0.51536(11) 0.42540(12) 0.0181(3) Uani 1.000000 .
H9 H 0.7755(2) 0.45746(11) 0.43465(12) 0.0217(4) Uiso 1.000000 R
C10 C 0.7927(2) 0.54776(12) 0.33937(12) 0.0176(3) Uani 1.000000 .
C11 C 0.7543(3) 0.62979(12) 0.31499(13) 0.0196(4) Uani 1.000000 .
C12 C 0.7746(3) 0.66041(13) 0.22901(14) 0.0229(4) Uani 1.000000 .
H12 H 0.7505(3) 0.71675(13) 0.21393(14) 0.0275(5) Uiso 1.000000 R
C13 C 0.8285(3) 0.60917(13) 0.16784(14) 0.0239(4) Uani 1.000000 .
H13 H 0.8413(3) 0.63044(13) 0.11029(14) 0.0286(5) Uiso 1.000000 R
C14 C 0.8661(2) 0.52494(13) 0.18810(13) 0.0208(4) Uani 1.000000 .
C15 C 0.9170(3) 0.47206(14) 0.12260(14) 0.0265(4) Uani 1.000000 .
H15 H 0.9258(3) 0.49352(14) 0.06452(14) 0.0318(5) Uiso 1.000000 R
C16 C 0.9537(3) 0.39066(14) 0.14153(15) 0.0291(5) Uani 1.000000 .
H16 H 0.9877(3) 0.35578(14) 0.09706(15) 0.0349(5) Uiso 1.000000 R
C17 C 0.9406(3) 0.35926(14) 0.22734(15) 0.0270(4) Uani 1.000000 .
H17 H 0.9665(3) 0.30278(14) 0.24077(15) 0.0324(5) Uiso 1.000000 R
C18 C 0.8908(3) 0.40880(12) 0.29242(13) 0.0224(4) Uani 1.000000 .
H18 H 0.8835(3) 0.38608(12) 0.35016(13) 0.0269(5) Uiso 1.000000 R
C19 C 0.8503(2) 0.49290(12) 0.27469(12) 0.0183(4) Uani 1.000000 .
C20 C 0.2547(4) 0.69313(17) 0.4342(3) 0.0549(9) Uani 1.000000 .
H20a H 0.2258(19) 0.7150(12) 0.4905(3) 0.0824(13) Uiso 1.000000 GR
H20b H 0.2754(11) 0.7390(9) 0.3950(14) 0.0824(13) Uiso 1.000000 GR
H20c H 0.1558(8) 0.6594(4) 0.4018(15) 0.0824(13) Uiso 1.000000 GR


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo O1 2.0093(14) . ?
Mo O2 1.9286(14) . ?
Mo O3 1.7046(15) . ?
Mo O4 1.6945(15) . ?
Mo O5 2.3456(14) . ?
Mo N2 2.2269(16) . ?
O1 C1 1.310(2) . ?
O2 C11 1.342(2) . ?
O5 C20 1.401(3) . ?
N1 N2 1.401(2) . ?
N1 C1 1.311(2) . ?
N2 C9 1.294(2) . ?
C1 C2 1.472(3) . ?
C2 C3 1.396(3) . ?
C2 C7 1.393(3) . ?
C3 C4 1.384(3) . ?
C4 C5 1.384(3) . ?
C5 C6 1.391(3) . ?
C6 C7 1.391(3) . ?
C6 C8 1.503(3) . ?
C9 C10 1.444(2) . ?
C10 C11 1.395(3) . ?
C10 C19 1.449(3) . ?
C11 C12 1.415(3) . ?
C12 C13 1.363(3) . ?
C13 C14 1.416(3) . ?
C14 C15 1.417(3) . ?
C14 C19 1.422(3) . ?
C15 C16 1.367(3) . ?
C16 C17 1.402(3) . ?
C17 C18 1.376(3) . ?
C18 C19 1.412(3) . ?

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
_geom_angle_publ_flag
O2 Mo O1 149.77(6) . . ?
O3 Mo O1 96.89(6) . . ?
O3 Mo O2 103.41(7) . . ?
O4 Mo O1 96.35(7) . . ?
O4 Mo O2 99.26(7) . . ?
O4 Mo O3 105.99(8) . . ?
O5 Mo O1 78.51(6) . . ?
O5 Mo O2 82.45(6) . . ?
O5 Mo O3 81.78(6) . . ?
O5 Mo O4 171.28(6) . . ?
N2 Mo O1 72.13(6) . . ?
N2 Mo O2 80.32(6) . . ?
N2 Mo O3 155.41(7) . . ?
N2 Mo O4 97.21(7) . . ?
N2 Mo O5 74.57(5) . . ?
C1 O1 Mo 120.22(12) . . ?
C11 O2 Mo 136.27(13) . . ?
C20 O5 Mo 124.88(15) . . ?
C1 N1 N2 109.62(15) . . ?
N1 N2 Mo 115.19(11) . . ?
C9 N2 Mo 128.85(13) . . ?
C9 N2 N1 115.96(15) . . ?
N1 C1 O1 122.70(17) . . ?
C2 C1 O1 117.50(16) . . ?
C2 C1 N1 119.78(17) . . ?
C3 C2 C1 120.03(18) . . ?
C7 C2 C1 120.44(17) . . ?
C7 C2 C3 119.54(18) . . ?
C4 C3 C2 119.2(2) . . ?
C5 C4 C3 120.7(2) . . ?
C6 C5 C4 121.15(19) . . ?
C7 C6 C5 117.9(2) . . ?
C8 C6 C5 121.3(2) . . ?
C8 C6 C7 120.8(2) . . ?
C6 C7 C2 121.55(19) . . ?
C10 C9 N2 124.51(17) . . ?
C11 C10 C9 121.12(17) . . ?
C19 C10 C9 119.45(17) . . ?
C19 C10 C11 119.30(17) . . ?
C10 C11 O2 123.24(17) . . ?
C12 C11 O2 115.77(17) . . ?
C12 C11 C10 120.93(18) . . ?
C13 C12 C11 120.07(18) . . ?
C14 C13 C12 121.50(18) . . ?
C15 C14 C13 120.68(18) . . ?
C19 C14 C13 119.64(18) . . ?
C19 C14 C15 119.68(19) . . ?
C16 C15 C14 121.13(19) . . ?
C17 C16 C15 119.2(2) . . ?
C18 C17 C16 121.2(2) . . ?
C19 C18 C17 120.99(19) . . ?
C14 C19 C10 118.54(17) . . ?
C18 C19 C10 123.67(17) . . ?
C18 C19 C14 117.79(18) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
