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_7124446
_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_moiety
'C53 H51 Mn N O P4, C32 H12 B F24, 2(C H2 Cl2)'
_chemical_formula_sum            'C87 H67 B Cl4 F24 Mn N O P4'
_chemical_formula_weight         1929.84
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2019-05-31T15:46:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-06-28 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                96.069(12)
_cell_angle_beta                 92.463(14)
_cell_angle_gamma                99.009(15)
_cell_formula_units_Z            2
_cell_length_a                   13.128(5)
_cell_length_b                   18.154(6)
_cell_length_c                   18.203(6)
_cell_measurement_reflns_used    9477
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      3.06
_cell_measurement_wavelength     0.71076
_cell_volume                     4253(3)
_computing_cell_refinement       'SAINT V8.38A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      -0.062603
_diffrn_orient_matrix_UB_12      -0.033712
_diffrn_orient_matrix_UB_13      0.013405
_diffrn_orient_matrix_UB_21      0.032442
_diffrn_orient_matrix_UB_22      0.000749
_diffrn_orient_matrix_UB_23      0.050792
_diffrn_orient_matrix_UB_31      -0.031571
_diffrn_orient_matrix_UB_32      0.04495
_diffrn_orient_matrix_UB_33      0.017215
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            153570
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.268
_diffrn_reflns_theta_min         2.906
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.534
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.08
_refine_ls_extinction_coef       0.0028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1206
_refine_ls_number_reflns         18945
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+9.4737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0
_reflns_number_gt                15989
_reflns_number_total             18945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06915a3.cif
_cod_data_source_block           shelx_CCDC3
_cod_original_cell_volume        4253(2)
_cod_database_code               7124446
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              55556