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_7124445
_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         'C54 H48 Mn O2 P4, C32 H12 B F24'
_chemical_formula_sum            'C86 H60 B F24 Mn O2 P4'
_chemical_formula_weight         1770.97
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      57
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_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             2019-04-02T16:29:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-07-01 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1290(11)
_cell_length_b                   18.6974(17)
_cell_length_c                   36.581(3)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.76
_cell_measurement_theta_min      2.23
_cell_measurement_wavelength     0.71073
_cell_volume                     8295.9(13)
_computing_cell_refinement       'SAINT V8.34A 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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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      -0.025036
_diffrn_orient_matrix_UB_12      -0.016537
_diffrn_orient_matrix_UB_13      -0.024636
_diffrn_orient_matrix_UB_21      0.030349
_diffrn_orient_matrix_UB_22      0.044624
_diffrn_orient_matrix_UB_23      -0.011216
_diffrn_orient_matrix_UB_31      0.072454
_diffrn_orient_matrix_UB_32      -0.024406
_diffrn_orient_matrix_UB_33      -0.003815
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            14403
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.001
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     540
_refine_ls_number_reflns         7645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0686
_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^)+(0.0779P)^2^+22.0432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1811
_reflns_Friedel_coverage         0
_reflns_number_gt                5136
_reflns_number_total             7645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06915a3.cif
_cod_data_source_block           shelx_CCDC2
_cod_database_code               7124445
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.993
_shelx_fab_checksum              47216
_shelx_res_checksum              65368