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_7227418
_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         '2(C40 H33 N2 O5 P2 Re), C H2 Cl2'
_chemical_formula_sum            'C81 H68 Cl2 N4 O10 P4 Re2'
_chemical_formula_weight         1824.57
_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
;
2016-12-19 deposited with the CCDC.
2017-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.081(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1714(7)
_cell_length_b                   46.877(3)
_cell_length_c                   17.9886(8)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.24
_cell_volume                     7415.1(8)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            85200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.546
_diffrn_reflns_theta_min         0.869
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.483
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.154
_refine_diff_density_max         2.311
_refine_diff_density_min         -1.857
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1131
_refine_ls_number_reflns         17490
_refine_ls_number_restraints     841
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0405P)^2^+49.4881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1234
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13096
_reflns_number_total             17490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra24421a2.cif
_cod_data_source_block           zj35mabs
_cod_database_code               7227418
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              72843