Carbene supported dimer of heavier ketenimine analogue with p and si atoms.
Roy, Sudipta; Dittrich, Birger; Mondal, Totan; Koley, Debasis; Stückl, A Claudia; Schwederski, Brigitte; Kaim, Wolfgang; John, Michael; Vasa, Suresh Kumar; Linser, Rasmus; Roesky, Herbert W.; Journal of the American Chemical Society 137 (2015) 6180–6183; doi:10.1021/jacs.5b03407

data_4123565
_publ_section_title
;
 Carbene supported dimer of heavier ketenimine analogue with p and si
 atoms.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6180
_journal_page_last               6183
_journal_paper_doi               10.1021/jacs.5b03407
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
;
2(C76 H116 N2 P2 Si2), 2(C6 H14), 2(C2.50 H2), C3 H7
;
_chemical_formula_sum            'C172 H271 N4 P4 Si4'
_chemical_formula_weight         2631.15
_chemical_name_common            {(cAAC)Si(P-Tip)}2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 93.599(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.5998(6)
_cell_length_b                   10.9274(5)
_cell_length_c                   46.7138(19)
_cell_measurement_temperature    100(2)
_cell_volume                     7947.4(6)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS, 2014)'
_computing_publication_material  'enCIFer 1.4, CCDC, 2011'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART 6000 Diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            158475
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.636
_diffrn_reflns_theta_min         1.895
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6263
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2014/1, multi-scan. (G. M. Sheldrick, 2014)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       block
_exptl_crystal_F_000             2894
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         14514
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0298P)^2^+6.3031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10710
_reflns_number_total             14514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b03407_si_002.cif
_cod_data_source_block           sr85
_cod_depositor_comments          'Adding full bibliography for 4123565.cif.'
_cod_database_code               4123565
_shelxl_version_number           2014/6
_shelx_res_checksum              48971
_shelx_hkl_checksum              94754