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_4133582
_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         'C55 H64 N4 O Si2'
_chemical_formula_sum            'C55 H64 N4 O Si2'
_chemical_formula_weight         853.28
_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     iterative
_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                83.107(3)
_cell_angle_beta                 84.228(3)
_cell_angle_gamma                66.911(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6253(4)
_cell_length_b                   12.9455(5)
_cell_length_c                   16.4249(5)
_cell_measurement_reflns_used    8482
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.4390
_cell_measurement_theta_min      2.6810
_cell_volume                     2447.40(15)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0217
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17249
_diffrn_reflns_theta_full        73.71
_diffrn_reflns_theta_max         73.71
_diffrn_reflns_theta_min         2.71
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27090
_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_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         9549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.6697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                8201
_reflns_number_total             9549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b11393_si_005.cif
_cod_data_source_block           cu-2961
_cod_original_cell_volume        2447.41(15)
_cod_database_code               4133582
_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:
 C11(H11), C16(H16), C17(H17), C18(H18), C19(H19), C24(H24), C25(H25),
 C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C34(H34), C35(H35), C37(H37),
  C39(H39), C42(H42), C46(H46), C47(H47), C49(H49), C51(H51), C54(H54),
 C56(H56), C58(H58)
2.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C)
;
_olex2_submission_special_instructions 'No special instructions were received'