A stable heavier group 14 analogue of vinylidene
Arnab Rit; Jesus Campos; Haoyu Niu; Simon Aldridge; Nature Chemistry 8 (2016) 1022–1026; doi:10.1038/nchem.2597

data_1552004
_publ_section_title
;
 A stable heavier group 14 analogue of vinylidene
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              1022
_journal_page_last               1026
_journal_paper_doi               10.1038/nchem.2597
_journal_volume                  8
_journal_year                    2016
_chemical_formula_moiety         'C26 H36 B N2, C7 H8, 0.5(Ge2 K2)'
_chemical_formula_sum            'C33 H44 B Ge K N2'
_chemical_formula_weight         591.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 108.53(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.718(5)
_cell_length_b                   18.519(4)
_cell_length_c                   14.938(3)
_cell_measurement_reflns_used    8067
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     7008(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14546
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.443
_diffrn_reflns_theta_min         5.206
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_platon_squeeze_details
;
The unit cell contains 4 toluene molecules which have 
been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.601
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7933
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0846P)^2^+9.3203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1797
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5286
_reflns_number_total             7933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2597-s5.cif
_cod_data_source_block           arnab018
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1552004
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              33627
_shelx_hkl_checksum              91263