Lewis Acid stabilization and Activation of Primary N-Nitrosamides
Chua, Zhijie; Rosadiuk, Kris; Perepichka, Inna; Bohle, Scott; RSC Adv.  (2017) –; doi:10.1039/C6RA24421A

data_7227417
_publ_section_title
;
 Lewis Acid stabilization and Activation of Primary N-Nitrosamides
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA24421A
_journal_year                    2017
_chemical_formula_moiety         'C40 H33 N2 O5 P2 Re'
_chemical_formula_sum            'C40 H33 N2 O5 P2 Re'
_chemical_formula_weight         869.82
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-12-19 deposited with the CCDC.
2017-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   44.728(3)
_cell_length_b                   44.728(3)
_cell_length_c                   12.0440(9)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.44
_cell_measurement_theta_min      2.19
_cell_volume                     20867(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            63501
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.040
_diffrn_reflns_theta_min         1.771
_exptl_absorpt_coefficient_mu    2.726
_exptl_absorpt_correction_T_max  0.8645
_exptl_absorpt_correction_T_min  0.4664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       rod
_exptl_crystal_F_000             7776
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.117
_refine_diff_density_max         2.631
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8142
_refine_ls_number_restraints     251
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0430P)^2^+99.3447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5851
_reflns_number_total             8142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra24421a2.cif
_cod_data_source_block           1435727
_cod_database_code               7227417
_shelxl_version_number           2014/6
_shelx_res_checksum              23016
_shelx_fab_checksum              22908