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#$Date: 2022-06-16 12:56:44 +0300 (Thu, 16 Jun 2022) $
#$Revision: 276068 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/54/8105429.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_8105429
loop_
_publ_author_name
'Lo, Kong Mun'
'Lee, See Mun'
'Tiekink, Edward R.T.'
_publ_section_title
;
 Crystal structure of
 (N,N-dimethylsulphoxide)-[N-(3-ethoxy-2-(oxide)benzylidene)-3-methoxybenzenecarbohydrazonato-κ3
 N,O,O′]-dioxo-molybdenum(VI), C19H22MoN2O7S
;
_journal_issue                   5
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1231
_journal_page_last               1233
_journal_paper_doi               10.1515/ncrs-2020-0281
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C19 H22 Mo N2 O7 S'
_chemical_formula_sum            'C19 H22 Mo N2 O7 S'
_chemical_formula_weight         518.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                81.451(2)
_cell_angle_beta                 72.444(2)
_cell_angle_gamma                87.930(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9719(2)
_cell_length_b                   10.3854(2)
_cell_length_c                   13.1042(3)
_cell_measurement_reflns_used    21260
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.4470
_cell_measurement_theta_min      3.5480
_cell_volume                     1022.85(4)
_computing_cell_refinement       'CrysAlisPro [1]'
_computing_data_collection       'CrysAlisPro [1]'
_computing_data_reduction        'CrysAlisPro [1]'
_computing_molecular_graphics    'ORTEP-3 for Windows [4]'
_computing_publication_material  'SHELXL-2018/3 [3]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXT 2014/5 [2]'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2558
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24067
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.049
_diffrn_reflns_theta_max         67.049
_diffrn_reflns_theta_min         3.575
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.602
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'CrysAlisPro [1]'
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0318P)²+1.0085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0503
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3660
_reflns_number_total             3664
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2020-0281_suppl.cif
_cod_data_source_block           shelx
_cod_database_code               8105429
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.352
_shelx_estimated_absorpt_t_max   0.536
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Mo Mo 0.63757(2) 0.52131(2) 0.22781(2) 0.00681(6) Uani 1 1 d . . . . .
S1 S 0.35944(5) 0.60157(4) 0.08143(3) 0.00964(9) Uani 1 1 d . . . . .
O1 O 0.72761(15) 0.70120(11) 0.22000(9) 0.0095(2) Uani 1 1 d . . . . .
O2 O 0.44349(16) 0.39946(12) 0.26529(10) 0.0121(3) Uani 1 1 d . . . . .
O3 O 1.02885(17) 1.12676(12) 0.07792(10) 0.0158(3) Uani 1 1 d . . . . .
O4 O 0.30680(17) 0.16869(12) 0.28011(10) 0.0143(3) Uani 1 1 d . . . . .
O5 O 0.75568(17) 0.44367(12) 0.30673(10) 0.0139(3) Uani 1 1 d . . . . .
O6 O 0.75092(16) 0.49783(12) 0.09827(10) 0.0131(3) Uani 1 1 d . . . . .
O7 O 0.45077(17) 0.65056(12) 0.15598(10) 0.0138(3) Uani 1 1 d . . . . .
N1 N 0.50584(19) 0.73704(14) 0.37379(12) 0.0099(3) Uani 1 1 d . . . . .
N2 N 0.46125(19) 0.61073(14) 0.36605(11) 0.0087(3) Uani 1 1 d . . . . .
C1 C 0.6469(2) 0.77439(16) 0.29460(13) 0.0090(3) Uani 1 1 d . . . . .
C2 C 0.3272(2) 0.55767(17) 0.44178(14) 0.0103(3) Uani 1 1 d . . . . .
H2 H 0.269685 0.605569 0.498753 0.012 Uiso 1 1 calc R U . . .
C3 C 0.2600(2) 0.42909(17) 0.44443(14) 0.0107(3) Uani 1 1 d . . . . .
C4 C 0.3193(2) 0.35610(17) 0.35869(14) 0.0102(3) Uani 1 1 d . . . . .
C5 C 0.2427(2) 0.23274(17) 0.36720(14) 0.0119(3) Uani 1 1 d . . . . .
C6 C 0.1089(2) 0.18586(18) 0.46033(15) 0.0154(4) Uani 1 1 d . . . . .
H6 H 0.056701 0.103271 0.465960 0.018 Uiso 1 1 calc R U . . .
C7 C 0.0506(2) 0.25867(18) 0.54533(15) 0.0157(4) Uani 1 1 d . . . . .
H7 H -0.040306 0.225286 0.608556 0.019 Uiso 1 1 calc R U . . .
C8 C 0.1242(2) 0.37857(18) 0.53802(14) 0.0127(4) Uani 1 1 d . . . . .
H8 H 0.083584 0.427837 0.596176 0.015 Uiso 1 1 calc R U . . .
C9 C 0.7209(2) 0.90563(16) 0.28371(14) 0.0096(3) Uani 1 1 d . . . . .
C10 C 0.8445(2) 0.95763(17) 0.18728(14) 0.0105(3) Uani 1 1 d . . . . .
H10 H 0.885136 0.907328 0.129816 0.013 Uiso 1 1 calc R U . . .
C11 C 0.9081(2) 1.08386(17) 0.17577(14) 0.0111(3) Uani 1 1 d . . . . .
C12 C 0.8502(2) 1.15780(17) 0.25960(15) 0.0129(4) Uani 1 1 d . . . . .
H12 H 0.893928 1.243801 0.251533 0.015 Uiso 1 1 calc R U . . .
C13 C 0.7271(2) 1.10421(18) 0.35587(15) 0.0150(4) Uani 1 1 d . . . . .
H13 H 0.686753 1.154527 0.413347 0.018 Uiso 1 1 calc R U . . .
C14 C 0.6630(2) 0.97915(17) 0.36879(15) 0.0128(3) Uani 1 1 d . . . . .
H14 H 0.580227 0.943322 0.434967 0.015 Uiso 1 1 calc R U . . .
C15 C 1.1074(3) 1.25225(18) 0.06526(16) 0.0172(4) Uani 1 1 d . . . . .
H15A H 1.016291 1.319053 0.071545 0.026 Uiso 1 1 calc R U . . .
H15B H 1.195254 1.269555 -0.006061 0.026 Uiso 1 1 calc R U . . .
H15C H 1.164495 1.254022 0.121628 0.026 Uiso 1 1 calc R U . . .
C16 C 0.2625(2) 0.03221(17) 0.29531(16) 0.0156(4) Uani 1 1 d . . . . .
H16A H 0.133539 0.020704 0.313662 0.019 Uiso 1 1 calc R U . . .
H16B H 0.301976 -0.015489 0.355084 0.019 Uiso 1 1 calc R U . . .
C17 C 0.3536(3) -0.01911(18) 0.19127(16) 0.0182(4) Uani 1 1 d . . . . .
H17A H 0.305435 0.022881 0.134240 0.027 Uiso 1 1 calc R U . . .
H17B H 0.334859 -0.113459 0.201222 0.027 Uiso 1 1 calc R U . . .
H17C H 0.479985 -0.000186 0.170530 0.027 Uiso 1 1 calc R U . . .
C18 C 0.1309(3) 0.6058(2) 0.15159(17) 0.0254(5) Uani 1 1 d . . . . .
H18A H 0.103717 0.541367 0.217195 0.038 Uiso 1 1 calc R U . . .
H18B H 0.062940 0.585427 0.104825 0.038 Uiso 1 1 calc R U . . .
H18C H 0.100001 0.692804 0.171420 0.038 Uiso 1 1 calc R U . . .
C19 C 0.3722(3) 0.73839(18) -0.02091(15) 0.0185(4) Uani 1 1 d . . . . .
H19A H 0.342784 0.817728 0.012768 0.028 Uiso 1 1 calc R U . . .
H19B H 0.288895 0.726219 -0.060560 0.028 Uiso 1 1 calc R U . . .
H19C H 0.491842 0.746293 -0.071098 0.028 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 0.0181 0.0091 '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 -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
O5 Mo O6 105.46(6) . .
O5 Mo O2 99.16(6) . .
O6 Mo O2 102.60(5) . .
O5 Mo O1 96.74(5) . .
O6 Mo O1 97.39(5) . .
O2 Mo O1 150.01(5) . .
O5 Mo N2 91.88(6) . .
O6 Mo N2 160.75(6) . .
O2 Mo N2 82.35(5) . .
O1 Mo N2 71.84(5) . .
O5 Mo O7 166.52(5) . .
O6 Mo O7 87.32(5) . .
O2 Mo O7 81.80(5) . .
O1 Mo O7 77.01(5) . .
N2 Mo O7 74.87(5) . .
O7 S1 C18 104.84(9) . .
O7 S1 C19 103.39(8) . .
C18 S1 C19 99.03(10) . .
C1 O1 Mo 119.99(10) . .
C4 O2 Mo 133.44(11) . .
C11 O3 C15 117.30(14) . .
C5 O4 C16 116.92(14) . .
S1 O7 Mo 121.58(7) . .
C1 N1 N2 108.84(14) . .
C2 N2 N1 116.32(14) . .
C2 N2 Mo 127.66(12) . .
N1 N2 Mo 115.95(10) . .
N1 C1 O1 123.36(15) . .
N1 C1 C9 119.69(15) . .
O1 C1 C9 116.94(15) . .
N2 C2 C3 123.51(16) . .
N2 C2 H2 118.2 . .
C3 C2 H2 118.2 . .
C4 C3 C8 119.61(16) . .
C4 C3 C2 123.37(16) . .
C8 C3 C2 117.00(16) . .
O2 C4 C3 123.18(16) . .
O2 C4 C5 117.29(16) . .
C3 C4 C5 119.48(16) . .
O4 C5 C6 124.71(16) . .
O4 C5 C4 115.77(15) . .
C6 C5 C4 119.52(16) . .
C5 C6 C7 120.77(17) . .
C5 C6 H6 119.6 . .
C7 C6 H6 119.6 . .
C8 C7 C6 120.23(17) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
C7 C8 C3 120.39(17) . .
C7 C8 H8 119.8 . .
C3 C8 H8 119.8 . .
C14 C9 C10 120.16(16) . .
C14 C9 C1 119.98(16) . .
C10 C9 C1 119.84(15) . .
C11 C10 C9 119.56(16) . .
C11 C10 H10 120.2 . .
C9 C10 H10 120.2 . .
O3 C11 C12 124.04(16) . .
O3 C11 C10 115.36(15) . .
C12 C11 C10 120.60(16) . .
C11 C12 C13 119.20(16) . .
C11 C12 H12 120.4 . .
C13 C12 H12 120.4 . .
C14 C13 C12 120.98(17) . .
C14 C13 H13 119.5 . .
C12 C13 H13 119.5 . .
C13 C14 C9 119.50(17) . .
C13 C14 H14 120.3 . .
C9 C14 H14 120.3 . .
O3 C15 H15A 109.5 . .
O3 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
O3 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
O4 C16 C17 107.62(15) . .
O4 C16 H16A 110.2 . .
C17 C16 H16A 110.2 . .
O4 C16 H16B 110.2 . .
C17 C16 H16B 110.2 . .
H16A C16 H16B 108.5 . .
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 . .
S1 C18 H18A 109.5 . .
S1 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
S1 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
S1 C19 H19A 109.5 . .
S1 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
S1 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo O5 1.7003(12) .
Mo O6 1.7145(12) .
Mo O2 1.9325(12) .
Mo O1 2.0029(12) .
Mo N2 2.2337(14) .
Mo O7 2.2872(12) .
S1 O7 1.5319(12) .
S1 C18 1.778(2) .
S1 C19 1.7860(18) .
O1 C1 1.324(2) .
O2 C4 1.348(2) .
O3 C11 1.373(2) .
O3 C15 1.432(2) .
O4 C5 1.362(2) .
O4 C16 1.443(2) .
N1 C1 1.304(2) .
N1 N2 1.397(2) .
N2 C2 1.292(2) .
C1 C9 1.475(2) .
C2 C3 1.448(2) .
C2 H2 0.9500 .
C3 C4 1.403(3) .
C3 C8 1.414(2) .
C4 C5 1.414(2) .
C5 C6 1.393(3) .
C6 C7 1.393(3) .
C6 H6 0.9500 .
C7 C8 1.374(3) .
C7 H7 0.9500 .
C8 H8 0.9500 .
C9 C14 1.399(2) .
C9 C10 1.394(2) .
C10 C11 1.393(2) .
C10 H10 0.9500 .
C11 C12 1.389(3) .
C12 C13 1.396(3) .
C12 H12 0.9500 .
C13 C14 1.381(3) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C17 1.504(3) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C18 S1 O7 Mo 117.60(10) . . . .
C19 S1 O7 Mo -139.10(9) . . . .
C1 N1 N2 C2 177.40(15) . . . .
C1 N1 N2 Mo -0.08(16) . . . .
N2 N1 C1 O1 1.1(2) . . . .
N2 N1 C1 C9 179.45(14) . . . .
Mo O1 C1 N1 -1.7(2) . . . .
Mo O1 C1 C9 179.87(11) . . . .
N1 N2 C2 C3 178.07(15) . . . .
Mo N2 C2 C3 -4.8(2) . . . .
N2 C2 C3 C4 -8.3(3) . . . .
N2 C2 C3 C8 173.58(16) . . . .
Mo O2 C4 C3 27.0(2) . . . .
Mo O2 C4 C5 -155.29(13) . . . .
C8 C3 C4 O2 177.47(16) . . . .
C2 C3 C4 O2 -0.6(3) . . . .
C8 C3 C4 C5 -0.2(2) . . . .
C2 C3 C4 C5 -178.27(16) . . . .
C16 O4 C5 C6 -15.0(2) . . . .
C16 O4 C5 C4 165.92(15) . . . .
O2 C4 C5 O4 1.7(2) . . . .
C3 C4 C5 O4 179.51(15) . . . .
O2 C4 C5 C6 -177.45(16) . . . .
C3 C4 C5 C6 0.3(3) . . . .
O4 C5 C6 C7 -179.53(16) . . . .
C4 C5 C6 C7 -0.4(3) . . . .
C5 C6 C7 C8 0.4(3) . . . .
C6 C7 C8 C3 -0.2(3) . . . .
C4 C3 C8 C7 0.1(3) . . . .
C2 C3 C8 C7 178.33(16) . . . .
N1 C1 C9 C14 13.0(2) . . . .
O1 C1 C9 C14 -168.59(15) . . . .
N1 C1 C9 C10 -165.08(16) . . . .
O1 C1 C9 C10 13.4(2) . . . .
C14 C9 C10 C11 -0.9(3) . . . .
C1 C9 C10 C11 177.16(15) . . . .
C15 O3 C11 C12 4.3(2) . . . .
C15 O3 C11 C10 -175.55(15) . . . .
C9 C10 C11 O3 -179.77(15) . . . .
C9 C10 C11 C12 0.4(3) . . . .
O3 C11 C12 C13 -179.90(16) . . . .
C10 C11 C12 C13 -0.1(3) . . . .
C11 C12 C13 C14 0.2(3) . . . .
C12 C13 C14 C9 -0.7(3) . . . .
C10 C9 C14 C13 1.0(3) . . . .
C1 C9 C14 C13 -176.99(16) . . . .
C5 O4 C16 C17 -177.34(14) . . . .
