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_1556495
_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            'C122 H132 Mg2 N4 P4'
_chemical_formula_weight         1826.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90.34(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.547(4)
_cell_length_b                   22.500(5)
_cell_length_c                   22.000(4)
_cell_measurement_reflns_used    69137
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.622
_cell_measurement_theta_min      1.342
_cell_volume                     10171(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_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     0.7107
_diffrn_reflns_av_R_equivalents  0.1103
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            68204
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         28.622
_diffrn_reflns_theta_min         1.342
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.9945
_exptl_absorpt_correction_T_min  0.9903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00449(19)
_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   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         12842
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0673P)^2^+10.2704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9091
_reflns_number_total             12842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cmpd2-.cif
_cod_data_source_block           compound_2-
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1556495
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              95742
_shelx_hkl_checksum              91579