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_1556483
_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         'C22 H26 N O2 P S Si'
_chemical_formula_sum            'C22 H26 N O2 P S Si'
_chemical_formula_weight         427.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                71.7520(10)
_cell_angle_beta                 70.2450(10)
_cell_angle_gamma                73.1050(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2087(4)
_cell_length_b                   10.5543(4)
_cell_length_c                   12.6990(5)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.75
_cell_volume                     1079.35(8)
_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)'
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_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  0.0192
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
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_diffrn_reflns_limit_l_min       -15
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.755
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6820
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs2008
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.290
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0290
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3473
_reflns_number_total             3796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2016-4-40.cif
_cod_data_source_block           sad
_cod_database_code               1556483
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              88838
_shelx_hkl_checksum              29887