Synthesis and Characterization of a Sulfonyl- and Iminophosphoryl-Functionalized Methanide and Methandiide
Feichtner, K.-S.; Gessner, V.H.; Inorganics 4 (2016) 40–; doi:10.3390/inorganics4040040

data_1556485
_publ_section_title
;
 Synthesis and Characterization of a Sulfonyl- and
 Iminophosphoryl-Functionalized Methanide and Methandiide
;
_journal_name_full               Inorganics
_journal_page_first              40
_journal_paper_doi               10.3390/inorganics4040040
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety
'C92 H106 Li8 N4 O9 P4 S4 Si4, C4 H10 O,O0.25 C2 H5'
_chemical_formula_sum            'C98 H121 Li8 N4 O10.5 P4 S4 Si4'
_chemical_formula_weight         1942.98
_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   geom
_cell_angle_alpha                90
_cell_angle_beta                 116.547(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.265(3)
_cell_length_b                   18.972(2)
_cell_length_c                   24.452(3)
_cell_measurement_reflns_used    7915
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      324.997
_cell_measurement_theta_min      1.442
_cell_volume                     10485(2)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-CCD'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1048
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            107435
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.442
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6957
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs2008
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       needle
_exptl_crystal_F_000             4100
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         18468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0375P)^2^+9.7593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11964
_reflns_number_total             18468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2016-4-40.cif
_cod_data_source_block           sad2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C98 H121 Li8 N4 O10.50 P4 S4 Si4'
_cod_database_code               1556485
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              79124
_shelx_hkl_checksum              78799