Pnictogen-Silicon Analogues of Benzene.
Seitz, Andreas E.; Eckhardt, Maria; Erlebach, Andreas; Peresypkina, Eugenia V.; Sierka, Marek; Scheer, Manfred; Journal of the American Chemical Society 138 (2016) 10433–10436; doi:10.1021/jacs.6b07389

data_4130840
_publ_section_title
;
 Pnictogen-Silicon Analogues of Benzene.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10433
_journal_page_last               10436
_journal_paper_doi               10.1021/jacs.6b07389
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C45 H69 N6 P3 Si3, (C5 H12)0.5'
_chemical_formula_structural     '((C15 H22 N2)3 Si3 P3) * 0.5(C5 H12)'
_chemical_formula_sum            'C47.5 H75 N6 P3 Si3'
_chemical_formula_weight         907.31
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 114.123(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4117(5)
_cell_length_b                   21.3974(4)
_cell_length_c                   25.7847(7)
_cell_measurement_reflns_used    27099
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.3360
_cell_measurement_theta_min      3.9900
_cell_volume                     10781.7(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.001
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.001
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57897
_diffrn_reflns_point_group_measured_fraction_full 1.001
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         73.481
_diffrn_reflns_theta_min         3.480
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.3581
_exptl_crystal_size_mid          0.1759
_exptl_crystal_size_min          0.0597
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1142
_refine_ls_number_reflns         20957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0624
_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^)+(0.1387P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16936
_reflns_number_total             20957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07389_si_002.cif
_cod_data_source_block           sean204
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C47.50 H75 N6 P3 Si3'
_cod_database_code               4130840
_shelxl_version_number           2013-2
_shelx_res_checksum              222
_shelx_hkl_checksum              57766