Triple Hydrogen Atom Abstraction from Mn-NH3 Complexes Results in Cyclophosphazenium Cations
Cook, Brian J.; Johnson, Samantha I.; Chambers, Geoffrey M.; Kaminsky, Werner; Bullock, R. Morris; Chemical Communications  (2019) –; doi:10.1039/C9CC06915A

data_7124442
_publ_section_title
;
 Triple Hydrogen Atom Abstraction from Mn-NH3 Complexes Results in
 Cyclophosphazenium Cations
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06915A
_journal_year                    2019
_chemical_formula_sum            'C25 H24 N2 O6 S'
_chemical_formula_weight         480.52
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc230vvv
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-06-28 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.863(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9630(7)
_cell_length_b                   10.0358(9)
_cell_length_c                   28.017(3)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.41
_cell_measurement_theta_min      4.68
_cell_volume                     2237.8(4)
_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-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34888
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.403
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'Bruker-Nonius FR591 Cu rotating anode'
_exptl_absorpt_coefficient_mu    1.681
_exptl_absorpt_correction_T_max  0.5849
_exptl_absorpt_correction_T_min  0.4698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.224
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0044(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4110
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0479P)^2^+1.4410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4099
_reflns_number_total             4110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06915a3.cif
_cod_data_source_block           19070_a
_cod_original_cell_volume        2237.8(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7124442
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.535
_shelx_estimated_absorpt_t_max   0.705
_shelx_res_checksum              22389