Germyliumylidene [ClGe:]+and Germathionium [ClGe=S]+ Supported by 1,8-bis(Tributylphosphazenyl)naphthalene
Matthias Driess; Yun Xiong; Shenglai Yao; Andreas Berkefeld; Shigeyoshi Inoue; Chem.Commun. 48 (2012) 12198–; doi:10.1039/c2cc36926e

data_7108677
_publ_section_title
;
 Germyliumylidene [ClGe:]+and Germathionium [ClGe=S]+ Supported by
 1,8-bis(Tributylphosphazenyl)naphthalene
;
_journal_name_full               Chem.Commun.
_journal_page_first              12198
_journal_paper_doi               10.1039/c2cc36926e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C38 H68 Cl2 Ge N2 O P2'
_chemical_formula_weight         774.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.496(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4821(7)
_cell_length_b                   19.3868(8)
_cell_length_c                   19.0651(12)
_cell_measurement_reflns_used    3192
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4663
_cell_measurement_theta_min      3.4369
_cell_volume                     4486.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18231
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
;
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7853
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0531P)^2^+2.2592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                6011
_reflns_number_total             7853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc36926e.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      p21/n
_cod_database_code               7108677