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#$Date: 2021-10-07 10:28:59 +0300 (Thu, 07 Oct 2021) $
#$Revision: 269827 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/48/1564862.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_1564862
loop_
_publ_author_name
'Zhang, Cai-Xia'
'Fang, Duo-Wen'
'Wang, Jun-Ling'
'Jia, Ai-Quan'
'Zhang, Qian-Feng'
_publ_section_title
;
 Syntheses, characterizations, and reactivities of new
 1,4,7-trimethyl-l,4,7-triazacyclononane (Me3tacn) molybdenum and tungsten
 complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119599
_journal_paper_doi               10.1016/j.ica.2020.119599
_journal_volume                  507
_journal_year                    2020
_chemical_formula_sum            'C14 H27 F6 Mo N4 O2 P S2'
_chemical_formula_weight         588.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.546(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.795(3)
_cell_length_b                   23.024(8)
_cell_length_c                   12.557(4)
_cell_measurement_reflns_used    2039
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.78
_cell_measurement_theta_min      2.40
_cell_volume                     2252.8(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13920
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.541
_diffrn_reflns_theta_min         2.400
_exptl_absorpt_coefficient_mu    0.906
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.713
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0684
_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)+(0.1097P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.2077
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2803
_reflns_number_total             5151
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            5b.cif
_cod_data_source_block           P21N
_cod_original_cell_volume        2252.9(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1564862
_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.
;
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.854
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.68756(7) 0.12624(2) 0.27992(4) 0.0506(2) Uani 1 1 d . . . . .
S1 S 0.8059(3) 0.05635(7) 0.14643(13) 0.0583(5) Uani 1 1 d . . . . .
S2 S 0.7968(3) 0.03394(8) 0.36692(14) 0.0671(5) Uani 1 1 d . . . . .
O1 O 0.9925(8) 0.1714(3) 0.4168(5) 0.0911(18) Uani 1 1 d . . . . .
O2 O 0.9451(8) 0.1889(3) 0.1314(5) 0.0914(18) Uani 1 1 d . . . . .
N1 N 0.5168(8) 0.2044(2) 0.2292(5) 0.0692(17) Uani 1 1 d . . . . .
N2 N 0.5268(10) 0.1470(5) 0.4260(5) 0.101(3) Uani 1 1 d . . . . .
N3 N 0.4176(8) 0.0834(3) 0.2383(6) 0.0729(18) Uani 1 1 d . . . . .
N4 N 0.9269(8) -0.0433(2) 0.2305(5) 0.0606(15) Uani 1 1 d . . . . .
C1 C 0.5004(14) 0.2388(4) 0.3298(10) 0.111(4) Uani 1 1 d . . . . .
H1A H 0.6121 0.2534 0.3526 0.133 Uiso 1 1 calc R U . . .
H1B H 0.4251 0.2717 0.3169 0.133 Uiso 1 1 calc R U . . .
C2 C 0.4325(13) 0.2030(6) 0.4113(10) 0.122(4) Uani 1 1 d . . . . .
H2A H 0.3130 0.1947 0.3937 0.147 Uiso 1 1 calc R U . . .
H2B H 0.4366 0.2243 0.4780 0.147 Uiso 1 1 calc R U . . .
C3 C 0.3986(14) 0.0945(6) 0.4278(8) 0.122(4) Uani 1 1 d . . . . .
H3A H 0.4614 0.0595 0.4469 0.147 Uiso 1 1 calc R U . . .
H3B H 0.3149 0.1014 0.4821 0.147 Uiso 1 1 calc R U . . .
C4 C 0.3092(14) 0.0855(5) 0.3260(10) 0.117(4) Uani 1 1 d . . . . .
H4A H 0.2454 0.0494 0.3292 0.140 Uiso 1 1 calc R U . . .
H4B H 0.2270 0.1167 0.3148 0.140 Uiso 1 1 calc R U . . .
C5 C 0.3461(13) 0.1250(4) 0.1514(8) 0.093(3) Uani 1 1 d . . . . .
H5A H 0.4118 0.1200 0.0875 0.112 Uiso 1 1 calc R U . . .
H5B H 0.2282 0.1143 0.1341 0.112 Uiso 1 1 calc R U . . .
C6 C 0.3508(12) 0.1849(3) 0.1812(7) 0.084(3) Uani 1 1 d . . . . .
H6A H 0.2612 0.1920 0.2318 0.100 Uiso 1 1 calc R U . . .
H6B H 0.3252 0.2083 0.1185 0.100 Uiso 1 1 calc R U . . .
C7 C 0.5945(13) 0.2480(4) 0.1507(9) 0.109(4) Uani 1 1 d . . . . .
H7A H 0.5138 0.2787 0.1362 0.163 Uiso 1 1 calc R U . . .
H7B H 0.6201 0.2284 0.0856 0.163 Uiso 1 1 calc R U . . .
H7C H 0.6981 0.2641 0.1816 0.163 Uiso 1 1 calc R U . . .
C8 C 0.6321(15) 0.1460(8) 0.5277(7) 0.185(8) Uani 1 1 d . . . . .
H8A H 0.6657 0.1849 0.5464 0.278 Uiso 1 1 calc R U . . .
H8B H 0.7326 0.1227 0.5183 0.278 Uiso 1 1 calc R U . . .
H8C H 0.5653 0.1298 0.5836 0.278 Uiso 1 1 calc R U . . .
C9 C 0.4156(14) 0.0247(4) 0.1895(11) 0.135(5) Uani 1 1 d . . . . .
H9A H 0.4463 -0.0037 0.2426 0.202 Uiso 1 1 calc R U . . .
H9B H 0.4964 0.0234 0.1332 0.202 Uiso 1 1 calc R U . . .
H9C H 0.3026 0.0165 0.1610 0.202 Uiso 1 1 calc R U . . .
C10 C 0.8519(9) 0.0073(3) 0.2456(6) 0.0561(17) Uani 1 1 d . . . . .
C11 C 0.9618(11) -0.0644(3) 0.1242(7) 0.082(2) Uani 1 1 d . . . . .
H11A H 0.9850 -0.0320 0.0785 0.123 Uiso 1 1 calc R U . . .
H11B H 0.8638 -0.0853 0.0965 0.123 Uiso 1 1 calc R U . . .
H11C H 1.0596 -0.0897 0.1273 0.123 Uiso 1 1 calc R U . . .
C12 C 0.9628(11) -0.0819(4) 0.3176(7) 0.083(2) Uani 1 1 d . . . . .
H12A H 1.0072 -0.0601 0.3775 0.125 Uiso 1 1 calc R U . . .
H12B H 1.0461 -0.1101 0.2969 0.125 Uiso 1 1 calc R U . . .
H12C H 0.8592 -0.1013 0.3369 0.125 Uiso 1 1 calc R U . . .
C13 C 0.8769(10) 0.1569(3) 0.3609(6) 0.069(2) Uani 1 1 d . . . . .
C14 C 0.8459(11) 0.1659(3) 0.1851(7) 0.068(2) Uani 1 1 d . . . . .
P1 P 0.4759(3) 0.84628(8) 0.16090(14) 0.0559(5) Uani 1 1 d . . . . .
F1 F 0.6110(9) 0.8621(4) 0.2474(6) 0.176(4) Uani 1 1 d . . . . .
F2 F 0.3449(10) 0.8319(5) 0.0704(5) 0.187(4) Uani 1 1 d . . . . .
F3 F 0.6187(8) 0.8163(3) 0.0937(5) 0.121(2) Uani 1 1 d . . . . .
F4 F 0.3345(8) 0.8777(3) 0.2250(4) 0.136(3) Uani 1 1 d . . . . .
F5 F 0.4419(12) 0.7920(3) 0.2244(6) 0.176(3) Uani 1 1 d . . . . .
F6 F 0.5160(12) 0.9023(3) 0.0983(6) 0.176(3) Uani 1 1 d . . . . .
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'
S S 0.1246 0.1234 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
C13 Mo1 C14 70.1(3) . .
C13 Mo1 N2 85.9(3) . .
C14 Mo1 N2 138.8(3) . .
C13 Mo1 N1 106.8(3) . .
C14 Mo1 N1 80.6(3) . .
N2 Mo1 N1 74.7(3) . .
C13 Mo1 N3 160.5(3) . .
C14 Mo1 N3 129.0(3) . .
N2 Mo1 N3 76.3(3) . .
N1 Mo1 N3 76.3(2) . .
C13 Mo1 S1 107.4(2) . .
C14 Mo1 S1 69.3(2) . .
N2 Mo1 S1 151.8(3) . .
N1 Mo1 S1 122.10(17) . .
N3 Mo1 S1 85.76(16) . .
C13 Mo1 S2 80.4(2) . .
C14 Mo1 S2 116.3(2) . .
N2 Mo1 S2 90.8(2) . .
N1 Mo1 S2 163.02(18) . .
N3 Mo1 S2 91.82(16) . .
S1 Mo1 S2 67.97(6) . .
C10 S1 Mo1 90.6(2) . .
C10 S2 Mo1 90.4(2) . .
C6 N1 C1 114.1(7) . .
C6 N1 C7 107.0(6) . .
C1 N1 C7 103.8(7) . .
C6 N1 Mo1 111.4(4) . .
C1 N1 Mo1 103.8(5) . .
C7 N1 Mo1 116.7(5) . .
C2 N2 C8 112.0(9) . .
C2 N2 C3 110.8(8) . .
C8 N2 C3 108.1(9) . .
C2 N2 Mo1 110.9(6) . .
C8 N2 Mo1 112.3(6) . .
C3 N2 Mo1 102.3(5) . .
C4 N3 C9 110.9(8) . .
C4 N3 C5 108.6(8) . .
C9 N3 C5 105.8(7) . .
C4 N3 Mo1 111.2(6) . .
C9 N3 Mo1 118.0(5) . .
C5 N3 Mo1 101.4(5) . .
C10 N4 C12 121.1(6) . .
C10 N4 C11 121.4(6) . .
C12 N4 C11 117.2(6) . .
C2 C1 N1 110.0(8) . .
C2 C1 H1A 109.7 . .
N1 C1 H1A 109.7 . .
C2 C1 H1B 109.7 . .
N1 C1 H1B 109.7 . .
H1A C1 H1B 108.2 . .
C1 C2 N2 113.4(8) . .
C1 C2 H2A 108.9 . .
N2 C2 H2A 108.9 . .
C1 C2 H2B 108.9 . .
N2 C2 H2B 108.9 . .
H2A C2 H2B 107.7 . .
C4 C3 N2 112.8(8) . .
C4 C3 H3A 109.0 . .
N2 C3 H3A 109.0 . .
C4 C3 H3B 109.0 . .
N2 C3 H3B 109.0 . .
H3A C3 H3B 107.8 . .
N3 C4 C3 114.2(8) . .
N3 C4 H4A 108.7 . .
C3 C4 H4A 108.7 . .
N3 C4 H4B 108.7 . .
C3 C4 H4B 108.7 . .
H4A C4 H4B 107.6 . .
C6 C5 N3 114.0(7) . .
C6 C5 H5A 108.7 . .
N3 C5 H5A 108.7 . .
C6 C5 H5B 108.7 . .
N3 C5 H5B 108.7 . .
H5A C5 H5B 107.6 . .
C5 C6 N1 114.5(7) . .
C5 C6 H6A 108.6 . .
N1 C6 H6A 108.6 . .
C5 C6 H6B 108.6 . .
N1 C6 H6B 108.6 . .
H6A C6 H6B 107.6 . .
N1 C7 H7A 109.5 . .
N1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N2 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N3 C9 H9A 109.5 . .
N3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N4 C10 S2 124.6(5) . .
N4 C10 S1 124.3(5) . .
S2 C10 S1 111.0(4) . .
N4 C11 H11A 109.5 . .
N4 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N4 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N4 C12 H12A 109.5 . .
N4 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N4 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O1 C13 Mo1 173.8(7) . .
O2 C14 Mo1 177.4(7) . .
F5 P1 F1 87.1(5) . .
F5 P1 F2 95.2(5) . .
F1 P1 F2 177.4(5) . .
F5 P1 F6 178.1(5) . .
F1 P1 F6 91.0(5) . .
F2 P1 F6 86.7(5) . .
F5 P1 F4 88.6(4) . .
F1 P1 F4 90.3(4) . .
F2 P1 F4 90.9(4) . .
F6 P1 F4 91.8(4) . .
F5 P1 F3 93.3(4) . .
F1 P1 F3 90.1(4) . .
F2 P1 F3 88.6(4) . .
F6 P1 F3 86.4(4) . .
F4 P1 F3 178.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 C13 1.905(9) .
Mo1 C14 1.964(9) .
Mo1 N2 2.299(7) .
Mo1 N1 2.318(6) .
Mo1 N3 2.370(6) .
Mo1 S1 2.5166(18) .
Mo1 S2 2.527(2) .
S1 C10 1.713(7) .
S2 C10 1.708(7) .
O1 C13 1.176(9) .
O2 C14 1.166(9) .
N1 C6 1.482(9) .
N1 C1 1.499(11) .
N1 C7 1.541(11) .
N2 C2 1.494(14) .
N2 C8 1.499(11) .
N2 C3 1.568(14) .
N3 C4 1.407(12) .
N3 C9 1.483(10) .
N3 C5 1.546(11) .
N4 C10 1.318(8) .
N4 C12 1.431(9) .
N4 C11 1.454(9) .
C1 C2 1.426(15) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.453(14) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.430(11) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
P1 F5 1.509(6) .
P1 F1 1.536(7) .
P1 F2 1.543(6) .
P1 F6 1.548(7) .
P1 F4 1.560(5) .
P1 F3 1.574(6) .
