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_1556484
_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_sum            'C48 H58 K2 N2 O5 P2 S2 Si2'
_chemical_formula_weight         1003.40
_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                112.315(3)
_cell_angle_beta                 90.340(3)
_cell_angle_gamma                110.779(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2841(10)
_cell_length_b                   15.3705(14)
_cell_length_c                   16.8163(15)
_cell_measurement_reflns_used    7525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.998
_cell_measurement_theta_min      1.956
_cell_volume                     2489.2(4)
_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  0.0755
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37279
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.956
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs2008
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         8770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+1.1645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6524
_reflns_number_total             8770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2016-4-40.cif
_cod_data_source_block           platon_pl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               1556484
_shelx_res_checksum              43474
_shelx_hkl_checksum              55556