Unusual activation pathways of amines in the reactions with molybdenum pentachloride
Bartalucci, Niccolò; Bortoluzzi, Marco; Marchetti, Fabio; Pampaloni, Guido; Schoch, Silvia; Zacchini, Stefano; New J. Chem. 41 (2017) 4329–4340; doi:10.1039/C6NJ03992H

data_7056160
_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            'C12 H32 Cl9.6 Mo2 N2 O0.4'
_chemical_formula_weight         742.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8611(7)
_cell_length_b                   13.6266(7)
_cell_length_c                   14.1240(6)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2245
_cell_measurement_theta_min      2.5435
_cell_volume                     2667.7(2)
_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 0.993
_diffrn_measured_fraction_theta_max 0.994
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30112
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.544
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1504 (selected reflections only, before parameter refinement)
 R(int) =  0.0494 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_description       prism
_exptl_crystal_F_000             1474
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         2.147
_refine_diff_density_min         -2.430
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0803
_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/[\s^2^(Fo^2^)+99.2501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.1913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2770
_reflns_number_total             2888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03992h3.cif
_cod_data_source_block           7
_cod_original_formula_sum        'C12 H32 Cl9.60 Mo2 N2 O0.40'
_cod_database_code               7056160
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.790
_shelx_res_checksum              83818