Methanediide Formation via Hydrogen Elimination in Magnesium versus Aluminium Hydride Complexes of a Sterically Demanding Bis(iminophosphoranyl)methanediide
Sindlinger, C.P.; Lawrence, S.R.; Cordes, D.B.; Slawin, A.M.Z.; Stasch, A.; Inorganics 5 (2017) 29–; doi:10.3390/inorganics5020029

data_1556496
_publ_section_title
;
 Methanediide Formation via Hydrogen Elimination in Magnesium versus
 Aluminium Hydride Complexes of a Sterically Demanding
 Bis(iminophosphoranyl)methanediide
;
_journal_name_full               Inorganics
_journal_page_first              29
_journal_paper_doi               10.3390/inorganics5020029
_journal_volume                  5
_journal_year                    2017
_chemical_formula_sum            'C49 H57 Al N2 P2'
_chemical_formula_weight         762.88
_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
_cell_angle_alpha                90
_cell_angle_beta                 99.58(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.149(3)
_cell_length_b                   18.972(4)
_cell_length_c                   17.427(4)
_cell_measurement_reflns_used    76352
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.604
_cell_measurement_theta_min      1.571
_cell_volume                     4286.8(17)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'ADSC quantum 210r'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            75030
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.604
_diffrn_reflns_theta_min         1.571
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         10752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0485P)^2^+2.3692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10060
_reflns_number_total             10752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cmpd3.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        4286.8(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1556496
_shelx_estimated_absorpt_t_min   0.992
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              24898
_shelx_hkl_checksum              22305