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_7056159
_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            'C4 H7 Cl5 Mo N'
_chemical_formula_weight         342.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8263(17)
_cell_length_b                   8.2825(12)
_cell_length_c                   10.2388(15)
_cell_measurement_reflns_used    5841
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4955
_cell_measurement_theta_min      3.0025
_cell_volume                     1002.9(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10237
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.990
_diffrn_reflns_theta_min         3.003
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.6403
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1423 (selected reflections only, before parameter refinement)
 R(int) =  0.0584 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_description       prism
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 941 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2180
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0227
_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/[\s^2^(Fo^2^)+(0.0092P)^2^+0.3630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0398
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2096
_reflns_number_total             2180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03992h3.cif
_cod_data_source_block           1
_cod_database_code               7056159
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.640
_shelx_estimated_absorpt_t_max   0.747
_shelx_res_checksum              2210