Geometrically Compelled Disilene with λ<sup>4</sup>-Coordinate Si<sup>II</sup> Atoms.
Kostenko, Arseni; Driess, Matthias; Journal of the American Chemical Society 140 (2018) 16962–16966; doi:10.1021/jacs.8b11393

data_4133585
_publ_section_title
;
 Geometrically Compelled Disilene with \l<sup>4</sup>-Coordinate
 Si<sup>II</sup> Atoms.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16962
_journal_page_last               16966
_journal_paper_doi               10.1021/jacs.8b11393
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C56 H64 N4 Si2'
_chemical_formula_sum            'C56 H64 N4 Si2'
_chemical_formula_weight         849.29
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                76.133(5)
_cell_angle_beta                 88.079(4)
_cell_angle_gamma                67.359(6)
_cell_formula_units_Z            2
_cell_length_a                   10.5082(6)
_cell_length_b                   13.0458(8)
_cell_length_c                   19.4480(10)
_cell_measurement_reflns_used    3330
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3990
_cell_measurement_theta_min      3.7650
_cell_volume                     2383.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.1032
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17144
_diffrn_reflns_theta_full        73.65
_diffrn_reflns_theta_max         73.65
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         9325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                5859
_reflns_number_total             9325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b11393_si_004.cif
_cod_data_source_block           cu-2934
_cod_original_cell_volume        2383.8(2)
_cod_database_code               4133585
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C13(H13), C19(H19), C21(H21), C23(H23), C25(H25), C28(H28),
 C29(H29), C32(H32), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C42(H42),
  C46(H46), C47(H47), C49(H49), C50(H50), C52(H52), C53(H53), C55(H55), C59(H59)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C41(H41A,H41B,
 H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C48(H48A,
 H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C60(H60A,H60B,H60C)
;
_olex2_submission_special_instructions 'No special instructions were received'