Experimental and Computational Study of Auxiliary Molecular Effects on the Mechanism of the Addition of Hydrazines to a Low-Valent Germanium Complex
Brown, Zachary D.; Guo, Jing-Dong; Nagase, Shigeru; Power, Philip P.; Organometallics 31 (2012) 3768–; doi:10.1021/om300271c

data_4078306
_publ_section_title
;
 Experimental and Computational Study of Auxiliary Molecular Effects on
 the Mechanism of the Addition of Hydrazines to a Low-Valent Germanium
 Complex
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3768
_journal_paper_doi               10.1021/om300271c
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C50 H58 Ge0.96 N2'
_chemical_formula_weight         756.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.9994(8)
_cell_length_b                   30.2957(13)
_cell_length_c                   14.1667(6)
_cell_measurement_reflns_used    6233
_cell_measurement_temperature    87(2)
_cell_measurement_theta_max      71.02
_cell_measurement_theta_min      4.16
_cell_volume                     8154.4(6)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2010-11.3) (Bruker, 2010)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      87(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker Duo APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45025
_diffrn_reflns_theta_full        71.57
_diffrn_reflns_theta_max         71.57
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.9177
_exptl_absorpt_correction_T_min  0.8092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3221
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7631
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0880P)^2^+17.0257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                6245
_reflns_number_total             7631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300271c_si_002.cif
_cod_data_source_block           pccn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               4078306