Syntheses and Reactions of Derivatives of (Pyrrolylaldiminato)germanium(II) and -Aluminum(III)
Yang, Ying; Zhao, Na; Zhu, Hongping; Roesky, Herbert W.; Organometallics 31 (2012) 1958–; doi:10.1021/om201252k

data_4076487
_publ_section_title
;
 Syntheses and Reactions of Derivatives of
 (Pyrrolylaldiminato)germanium(II) and -Aluminum(III)
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1958
_journal_paper_doi               10.1021/om201252k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C33 H47 Ge N3'
_chemical_formula_weight         558.33
_chemical_name_common            LGeN(H)Ar
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.827(3)
_cell_angle_beta                 113.792(3)
_cell_angle_gamma                91.080(2)
_cell_formula_units_Z            8
_cell_length_a                   18.4395(5)
_cell_length_b                   18.7543(6)
_cell_length_c                   21.2127(7)
_cell_measurement_reflns_used    25070
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.0458
_cell_measurement_theta_min      3.3391
_cell_volume                     6304.2(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41153
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    1.486
_exptl_absorpt_correction_T_max  0.8079
_exptl_absorpt_correction_T_min  0.5880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.271
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1365
_refine_ls_number_reflns         18427
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0601
_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^)+(0.1157P)^2^+14.3691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.2148
_reflns_number_gt                15121
_reflns_number_total             18427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201252k_si_002.cif
_cod_data_source_block           yy123
_cod_original_cell_volume        6304.1(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076487