#------------------------------------------------------------------------------
#$Date: 2025-08-04 09:03:09 +0200 (Mon 04 de Aug de 2025) $
#$Revision: 301442 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/61/7056161.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_7056161
loop_
_publ_author_name
'Bartalucci, Niccolò'
'Bortoluzzi, Marco'
'Marchetti, Fabio'
'Pampaloni, Guido'
'Schoch, Silvia'
'Zacchini, Stefano'
_publ_section_title
;
 Unusual activation pathways of amines in the reactions with molybdenum
 pentachloride
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              4329
_journal_page_last               4340
_journal_paper_doi               10.1039/C6NJ03992H
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C43 H42 Cl8 Mo N2'
_chemical_formula_weight         966.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-30 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.818(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0833(9)
_cell_length_b                   13.2029(10)
_cell_length_c                   16.6033(12)
_cell_measurement_reflns_used    3427
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.4345
_cell_measurement_theta_min      2.5265
_cell_volume                     2146.4(3)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2415
_diffrn_reflns_av_unetI/netI     0.1445
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30144
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.994
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_correction_T_min  0.8918
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1219 (selected reflections only, before parameter refinement)
 R(int) =  0.0768 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.530
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3791
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1822
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0834P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1622
_reflns_number_total             3791
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6nj03992h3.cif
_cod_data_source_block           6
_cod_database_code               7056161
#BEGIN Tags that were not found in dictionaries:
_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   0.892
_shelx_estimated_absorpt_t_max   0.921
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 1.0000 0.5000 0.5000 0.0565(4) Uani 1 2 d S . P . .
Cl1 Cl 0.8005(3) 0.41974(18) 0.42234(13) 0.0742(8) Uani 1 1 d . . . . .
Cl2 Cl 1.1016(3) 0.33933(16) 0.53285(13) 0.0701(7) Uani 1 1 d . . . . .
Cl3 Cl 1.0841(2) 0.50493(16) 0.37541(11) 0.0616(6) Uani 1 1 d . . . . .
N1 N 0.9488(8) 0.2006(5) 0.2684(4) 0.067(2) Uani 1 1 d . . . . .
C1 C 0.9495(9) 0.2901(6) 0.2132(5) 0.061(2) Uani 1 1 d . . . . .
H1A H 0.9842 0.3497 0.2480 0.073 Uiso 1 1 calc R U . . .
H1B H 1.0132 0.2765 0.1775 0.073 Uiso 1 1 calc R U . . .
C2 C 0.8360(11) 0.1675(9) 0.2848(7) 0.105(4) Uani 1 1 d . . . . .
H2 H 0.7535 0.2006 0.2583 0.126 Uiso 1 1 calc R U . . .
C3 C 1.0777(11) 0.1948(9) 0.3361(6) 0.098(4) Uani 1 1 d . . . . .
H3A H 1.0750 0.2490 0.3769 0.118 Uiso 1 1 calc R U . . .
H3B H 1.0788 0.1291 0.3651 0.118 Uiso 1 1 calc R U . . .
C11 C 0.8127(9) 0.3147(6) 0.1597(5) 0.050(2) Uani 1 1 d . . . . .
C12 C 0.7625(10) 0.2642(7) 0.0847(5) 0.064(3) Uani 1 1 d . . . . .
H12 H 0.8150 0.2118 0.0682 0.077 Uiso 1 1 calc R U . . .
C13 C 0.6383(11) 0.2896(8) 0.0347(6) 0.079(3) Uani 1 1 d . . . . .
H13 H 0.6056 0.2549 -0.0163 0.094 Uiso 1 1 calc R U . . .
C14 C 0.5607(11) 0.3647(9) 0.0577(7) 0.086(3) Uani 1 1 d . . . . .
H14 H 0.4745 0.3825 0.0230 0.103 Uiso 1 1 calc R U . . .
C15 C 0.6109(11) 0.4142(7) 0.1326(7) 0.079(3) Uani 1 1 d . . . . .
H15 H 0.5581 0.4662 0.1494 0.095 Uiso 1 1 calc R U . . .
C16 C 0.7350(10) 0.3893(7) 0.1824(5) 0.064(2) Uani 1 1 d . . . . .
H16 H 0.7676 0.4241 0.2334 0.077 Uiso 1 1 calc R U . . .
C21 C 0.8264(9) 0.0830(7) 0.3410(5) 0.065(3) Uani 1 1 d . . . . .
C22 C 0.7847(8) -0.0112(7) 0.3086(5) 0.059(2) Uani 1 1 d . . . . .
H22 H 0.7648 -0.0215 0.2503 0.071 Uiso 1 1 calc R U . . .
C23 C 0.7716(9) -0.0912(6) 0.3608(5) 0.059(2) Uani 1 1 d . . . . .
H23 H 0.7459 -0.1565 0.3384 0.070 Uiso 1 1 calc R U . . .
C24 C 0.7963(9) -0.0751(7) 0.4453(5) 0.060(2) Uani 1 1 d . . . . .
H24 H 0.7890 -0.1294 0.4815 0.073 Uiso 1 1 calc R U . . .
C25 C 0.8315(11) 0.0204(7) 0.4766(5) 0.079(3) Uani 1 1 d . . . . .
H25 H 0.8452 0.0319 0.5345 0.094 Uiso 1 1 calc R U . . .
C26 C 0.8472(11) 0.0995(7) 0.4256(6) 0.082(3) Uani 1 1 d . . . . .
H26 H 0.8721 0.1648 0.4482 0.098 Uiso 1 1 calc R U . . .
C31 C 1.2073(10) 0.2045(8) 0.3090(6) 0.064(3) Uani 1 1 d . . . . .
C32 C 1.3018(13) 0.2767(7) 0.3470(6) 0.081(3) Uani 1 1 d . . . . .
H32 H 1.2827 0.3214 0.3876 0.097 Uiso 1 1 calc R U . . .
C33 C 1.4282(13) 0.2816(9) 0.3232(7) 0.090(3) Uani 1 1 d . . . . .
H33 H 1.4955 0.3300 0.3476 0.108 Uiso 1 1 calc R U . . .
C34 C 1.4515(13) 0.2152(10) 0.2644(8) 0.099(4) Uani 1 1 d . . . . .
H34 H 1.5372 0.2166 0.2501 0.119 Uiso 1 1 calc R U . . .
C35 C 1.3554(17) 0.1475(11) 0.2261(8) 0.116(5) Uani 1 1 d . . . . .
H35 H 1.3717 0.1048 0.1834 0.139 Uiso 1 1 calc R U . . .
C36 C 1.2365(15) 0.1419(8) 0.2496(7) 0.091(4) Uani 1 1 d . . . . .
H36 H 1.1708 0.0929 0.2242 0.109 Uiso 1 1 calc R U . . .
C101 C 0.414(3) 0.036(2) 0.0207(13) 0.150 Uiso 0.5 1 d D U P A -1
H10A H 0.3279 0.0100 0.0310 0.180 Uiso 0.5 1 calc R U P A -1
H10B H 0.3987 0.1049 -0.0041 0.180 Uiso 0.5 1 calc R U P A -1
Cl11 Cl 0.5506(8) 0.0355(6) 0.1134(6) 0.136(3) Uani 0.5 1 d D . P A -1
Cl12 Cl 0.4841(11) -0.0465(9) -0.0410(7) 0.168(4) Uani 0.5 1 d D . P A -1
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'
Cl Cl 0.1484 0.1585 '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'
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
Cl2 Mo1 Cl2 180.00(12) 3_766 .
Cl2 Mo1 Cl1 89.38(9) 3_766 3_766
Cl2 Mo1 Cl1 90.62(9) . 3_766
Cl2 Mo1 Cl1 90.62(9) 3_766 .
Cl2 Mo1 Cl1 89.38(9) . .
Cl1 Mo1 Cl1 180.0 3_766 .
Cl2 Mo1 Cl3 89.99(7) 3_766 .
Cl2 Mo1 Cl3 90.01(7) . .
Cl1 Mo1 Cl3 91.59(8) 3_766 .
Cl1 Mo1 Cl3 88.41(8) . .
Cl2 Mo1 Cl3 90.01(7) 3_766 3_766
Cl2 Mo1 Cl3 89.99(7) . 3_766
Cl1 Mo1 Cl3 88.41(8) 3_766 3_766
Cl1 Mo1 Cl3 91.59(8) . 3_766
Cl3 Mo1 Cl3 180.0 . 3_766
C2 N1 C1 121.6(8) . .
C2 N1 C3 117.9(7) . .
C1 N1 C3 111.6(7) . .
C11 C1 N1 113.5(7) . .
C11 C1 H1A 108.9 . .
N1 C1 H1A 108.9 . .
C11 C1 H1B 108.9 . .
N1 C1 H1B 108.9 . .
H1A C1 H1B 107.7 . .
N1 C2 C21 125.3(9) . .
N1 C2 H2 117.3 . .
C21 C2 H2 117.3 . .
C31 C3 N1 115.8(8) . .
C31 C3 H3A 108.3 . .
N1 C3 H3A 108.3 . .
C31 C3 H3B 108.3 . .
N1 C3 H3B 108.3 . .
H3A C3 H3B 107.4 . .
C16 C11 C12 118.7(8) . .
C16 C11 C1 120.2(8) . .
C12 C11 C1 121.1(8) . .
C13 C12 C11 120.6(9) . .
C13 C12 H12 119.7 . .
C11 C12 H12 119.7 . .
C12 C13 C14 120.5(9) . .
C12 C13 H13 119.7 . .
C14 C13 H13 119.7 . .
C13 C14 C15 118.6(9) . .
C13 C14 H14 120.7 . .
C15 C14 H14 120.7 . .
C16 C15 C14 121.0(9) . .
C16 C15 H15 119.5 . .
C14 C15 H15 119.5 . .
C15 C16 C11 120.6(9) . .
C15 C16 H16 119.7 . .
C11 C16 H16 119.7 . .
C22 C21 C26 119.6(8) . .
C22 C21 C2 119.7(9) . .
C26 C21 C2 120.4(9) . .
C21 C22 C23 120.4(7) . .
C21 C22 H22 119.8 . .
C23 C22 H22 119.8 . .
C24 C23 C22 119.6(8) . .
C24 C23 H23 120.2 . .
C22 C23 H23 120.2 . .
C25 C24 C23 119.5(8) . .
C25 C24 H24 120.3 . .
C23 C24 H24 120.3 . .
C24 C25 C26 121.3(8) . .
C24 C25 H25 119.4 . .
C26 C25 H25 119.4 . .
C25 C26 C21 119.5(9) . .
C25 C26 H26 120.3 . .
C21 C26 H26 120.3 . .
C36 C31 C32 119.9(11) . .
C36 C31 C3 121.4(11) . .
C32 C31 C3 118.7(11) . .
C31 C32 C33 117.9(11) . .
C31 C32 H32 121.0 . .
C33 C32 H32 121.0 . .
C34 C33 C32 119.0(11) . .
C34 C33 H33 120.5 . .
C32 C33 H33 120.5 . .
C35 C34 C33 121.9(13) . .
C35 C34 H34 119.0 . .
C33 C34 H34 119.0 . .
C36 C35 C34 118.9(13) . .
C36 C35 H35 120.5 . .
C34 C35 H35 120.5 . .
C35 C36 C31 122.3(12) . .
C35 C36 H36 118.9 . .
C31 C36 H36 118.9 . .
Cl12 C101 Cl11 99.4(12) . .
Cl12 C101 H10A 111.9 . .
Cl11 C101 H10A 111.9 . .
Cl12 C101 H10B 111.9 . .
Cl11 C101 H10B 111.9 . .
H10A C101 H10B 109.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 Cl2 2.362(2) 3_766
Mo1 Cl2 2.362(2) .
Mo1 Cl1 2.365(2) 3_766
Mo1 Cl1 2.365(2) .
Mo1 Cl3 2.4169(17) .
Mo1 Cl3 2.4169(17) 3_766
N1 C2 1.306(11) .
N1 C1 1.496(10) .
N1 C3 1.504(11) .
C1 C11 1.487(11) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C21 1.473(12) .
C2 H2 0.9500 .
C3 C31 1.486(13) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C11 C16 1.367(11) .
C11 C12 1.396(10) .
C12 C13 1.368(11) .
C12 H12 0.9500 .
C13 C14 1.373(13) .
C13 H13 0.9500 .
C14 C15 1.389(13) .
C14 H14 0.9500 .
C15 C16 1.365(13) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C21 C22 1.380(11) .
C21 C26 1.386(11) .
C22 C23 1.393(11) .
C22 H22 0.9500 .
C23 C24 1.382(10) .
C23 H23 0.9500 .
C24 C25 1.377(12) .
C24 H24 0.9500 .
C25 C26 1.378(12) .
C25 H25 0.9500 .
C26 H26 0.9500 .
C31 C36 1.372(14) .
C31 C32 1.388(12) .
C32 C33 1.423(14) .
C32 H32 0.9500 .
C33 C34 1.373(15) .
C33 H33 0.9500 .
C34 C35 1.359(16) .
C34 H34 0.9500 .
C35 C36 1.349(16) .
C35 H35 0.9500 .
C36 H36 0.9500 .
C101 Cl12 1.757(17) .
C101 Cl11 1.803(18) .
C101 H10A 0.9900 .
C101 H10B 0.9900 .
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
C2 N1 C1 C11 -18.6(13)
C3 N1 C1 C11 -165.1(8)
C1 N1 C2 C21 -177.3(9)
C3 N1 C2 C21 -32.8(17)
C2 N1 C3 C31 163.0(10)
C1 N1 C3 C31 -49.2(12)
N1 C1 C11 C16 98.1(9)
N1 C1 C11 C12 -83.4(10)
C16 C11 C12 C13 0.5(13)
C1 C11 C12 C13 -178.0(8)
C11 C12 C13 C14 -0.3(15)
C12 C13 C14 C15 -0.1(16)
C13 C14 C15 C16 0.3(16)
C14 C15 C16 C11 -0.1(15)
C12 C11 C16 C15 -0.3(13)
C1 C11 C16 C15 178.2(8)
N1 C2 C21 C22 -100.8(13)
N1 C2 C21 C26 84.9(16)
C26 C21 C22 C23 -3.9(14)
C2 C21 C22 C23 -178.3(9)
C21 C22 C23 C24 2.1(13)
C22 C23 C24 C25 1.0(14)
C23 C24 C25 C26 -2.3(15)
C24 C25 C26 C21 0.4(17)
C22 C21 C26 C25 2.7(15)
C2 C21 C26 C25 177.0(10)
N1 C3 C31 C36 -55.3(13)
N1 C3 C31 C32 126.8(9)
C36 C31 C32 C33 -1.0(13)
C3 C31 C32 C33 176.9(8)
C31 C32 C33 C34 -0.2(14)
C32 C33 C34 C35 2.5(18)
C33 C34 C35 C36 -3.5(19)
C34 C35 C36 C31 2.3(18)
C32 C31 C36 C35 0.0(16)
C3 C31 C36 C35 -177.9(10)
